CN103113139B - Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge - Google Patents
Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge Download PDFInfo
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- CN103113139B CN103113139B CN201310069651.1A CN201310069651A CN103113139B CN 103113139 B CN103113139 B CN 103113139B CN 201310069651 A CN201310069651 A CN 201310069651A CN 103113139 B CN103113139 B CN 103113139B
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Abstract
The invention discloses a method for producing a multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge. The method is characterized by comprising the following steps of: adding wet-process phosphoric acid raffinate acid, sludge acid and de-magging sludge to a reactor; fully mixing and evenly agitating, adding 65-58% of nitric acid to the reactor to react for 5-10minutes; adding ammonia to the reactor to neutralize, controlling the pH of the material at 5.0-6.5, and finally obtaining slurry of nitric phosphate. The method for producing the multivariate nitro compound fertilizer from the wet-process phosphoric acid purification sludge has the characteristics of being simple in process, low in energy consumption, low in cost and high in obtained product value; the wet-process phosphoric acid purified waste and the waste for industrially producing ammonium dihydrogen phosphate can be fully and repeatedly utilized; the waste is changed into precious resource to obtain a product with high value; the energy source is saved; and industrial pollution is greatly reduced.
Description
Technical field
The invention belongs to composite fertilizer's manufacturing technology field, specifically, relate to a kind of method that wet phosphoric acid purifying sludge produces polynary nitro-compound fertilizer.
Background technology
After the purification of phosphoric acid by wet process extraction agent, remaining acid is called as raffinate, and its main component is the P of 18 ~ 22%
2o
5, and a large amount of impurity.Along with the consumption of high-quality phosphate rock resource, phosphorus ore grade is more and more lower, and in raffinate, foreign matter content is more and more higher.Existing industrial ammonium phosphate device is difficult to these raffinates of digestion.In Chinese patent CN102161602A disclosed in 24 days Augusts in 2011, relate to a kind of by-product raffinate of phosphoric acid purification in a wet process and High-Mg phosphate tailings slag is the method that phosphorus magnesium compound fertilizer prepared by raw material, although this method can process raffinate, P in its raffinate used
2o
5content is 42 ~ 46%, belongs to the waste to phosphor resource with this method process raffinate, does not promote its due value.
Utilize phosphoric acid what slag to produce the flow process of powdery monoammonium phosphate in prior art, adopt the quick ammonification neutralization of pump circulation, two-effect evaporation concentrates, drying process with atomizing, dilute phosphoric acid [design: w(P
2o
5) 24% ~ 26%, w(solid) 4% ~ 6%] react with gas ammonia in the quick ammoniation reactor of pump circulation, and the neutralization that constantly circulates in endless tube outside; Slip after neutralization first after through II effect, I effect evaporation concentration, then send into drying tower through high-pressure pump, by controlling the water content controlling into drying tower slip into the quantity of steam of I effect well heater, slip w(H
2o) control 22% ~ 25%; Through high-pressure pump send into drying tower slip through pressure nozzle atomization after, from top to bottom with hot gas flow counter current contact while dried, the qualified powdery finished product generated after hot gas flow drying.But this flow process is oversize, and there is two-step enrichment process that energy consumption and cost are increased.
Nowadays a large amount of chemical slags can also be produced in industrial ammonium phosphate production process, but its P
2o
5content is between 20 ~ 23%.If do not processed it, not only can cause the pollution of environment, but also the waste of resource can be caused.
The shortcoming of prior art: the method for existing process raffinate and phosphoric acid sludge all also exists the problem that energy consumption is high, cost is high, the output value is low.
Summary of the invention
For solving above technical problem, the object of the present invention is to provide that a kind of technique is simple, energy consumption is low, cost is low and products obtained therefrom costly wet phosphoric acid purifying sludge produces the method for polynary nitro-compound fertilizer.
The present invention seeks to realize like this: a kind of wet phosphoric acid purifying sludge produces the method for polynary nitro-compound fertilizer, and its key is to comprise the following steps:
(1) will be 18 ~ 22%P containing massfraction
2o
5phosphoric acid by wet process raffinate, be 20 ~ 23%P containing massfraction
2o
5slag acid and containing massfraction be 20 ~ 23%P
2o
5chemical de-magging slag, be 100 ~ 110 parts, 100 ~ 104 parts and 110 ~ 119 parts by mass fraction respectively and join in reactor, fully mix and stir;
(2) in reactor, add mass fraction be again 300 ~ 350 parts of concentration is the nitric acid of 65 ~ 68%, reaction 5 ~ 10min;
(3) in reactor, then add the ammonia neutralization that mass fraction is 95 ~ 105 parts, the pH of material is controlled between 5.0 ~ 6.5, finally obtains the slip of nitrophosphate fertilizer.
Direct for the slip of above-mentioned nitrophosphate fertilizer spray granulating obtained the nitrophosphate fertilizer of granular high-nitrate state nitrogen content, maybe this slip is directly dried at 100 ~ 105 DEG C, pulverize the nitrophosphate fertilizer obtaining powdery high-nitrate state nitrogen content.
Above-mentioned slag acid and chemical de-magging slag are the by product of manufacture phosphorus ammonium.
Beneficial effect:
A kind of wet phosphoric acid purifying of the present invention sludge produces the method for polynary nitro-compound fertilizer, have that technique is simple, energy consumption is low, cost is low and products obtained therefrom is worth high, the waste material of the waste material of wet phosphoric acid purifying and industrial production phosphorus ammonium fully can be reused, turn waste into wealth, obtain costly product, save the energy, greatly reduce industrial pollution.
Embodiment
Embodiment 1:
Wet phosphoric acid purifying sludge produces a method for polynary nitro-compound fertilizer, comprises the following steps:
(1) adding 100 parts containing massfraction to reactor is 18 ~ 22%P
2o
5phosphoric acid by wet process raffinate, 100 parts containing massfraction be 20 ~ 23%P
2o
5manufacture phosphorus ammonium slag acid and 119 parts contain massfraction be 20 ~ 23%P
2o
5the chemical de-magging slag of manufacture phosphorus ammonium, fully mix and stir.
(2) in reactor, adding 350 parts of concentration again is the nitric acid of 65 ~ 68%, reaction 10min.
(3) in reactor, add 105 parts of ammonia neutralizations, the pH controlling material, 5.0, namely obtains the slip of nitrophosphate fertilizer.
(4) the direct spray granulating of the slip obtained just can obtain the nitrophosphate fertilizer of granular high-nitrate state nitrogen content, and (total nitrogen content is 26%, P
2o
5content is 12%, and wherein nitrate content is 12%).
Embodiment 2:
Wet phosphoric acid purifying sludge produces a method for polynary nitro-compound fertilizer, comprises the following steps:
(1) adding 107 parts containing massfraction to reactor is 18 ~ 22%P
2o
5phosphoric acid by wet process raffinate, 104 parts containing massfraction be 20 ~ 23%P
2o
5manufacture phosphorus ammonium slag acid and 110 parts contain massfraction be 20 ~ 23%P
2o
5the chemical de-magging slag of manufacture phosphorus ammonium, fully mix and stir.
(2) in reactor, adding 300 parts of concentration again is the nitric acid of 65 ~ 68%, reaction 10min.
(3) in reactor, add 95 parts of ammonia neutralizations, the pH controlling material, 5.0, namely obtains the slip of nitrophosphate fertilizer.
(4) the direct spray granulating of the slip obtained just can obtain the nitrophosphate fertilizer of granular high-nitrate state nitrogen content, and (total nitrogen content is 25%, P
2o
5content is 13.5%, and wherein nitrate content is 11%).
Embodiment 3:
Wet phosphoric acid purifying sludge produces a method for polynary nitro-compound fertilizer, comprises the following steps:
(1) 105 parts of P are added to reactor
2o
5massfraction is phosphoric acid by wet process raffinate, 104 parts of P of 18 ~ 22%
2o
5massfraction is slag acid and 112 parts of P of the manufacture phosphorus ammonium of 20 ~ 23%
2o
5massfraction is the chemical de-magging slag of the manufacture phosphorus ammonium of 20 ~ 23%, fully mixes and stirs.
(2) in reactor, adding 300 parts of concentration again is the nitric acid of 65 ~ 68%, reaction 10min.
(3) in reactor, add 105 parts of ammonia neutralizations, the pH controlling material, 6.5, namely obtains the slip of nitrophosphate fertilizer.
(4) slip obtained is dried at 100 DEG C, and pulverizing is powdery nitrophosphate fertilizer, and (total nitrogen content is 26%, P
2o
5content is 12.5%, and wherein nitrate content is 10.5%).
Embodiment 4:
Wet phosphoric acid purifying sludge produces a method for polynary nitro-compound fertilizer, comprises the following steps:
(1) 102 parts of P are added to reactor
2o
5massfraction is phosphoric acid by wet process raffinate, 100 parts of P of 18 ~ 22%
2o
5massfraction is slag acid and 118 parts of P of the manufacture phosphorus ammonium of 20 ~ 23%
2o
5massfraction is the chemical de-magging slag of the manufacture phosphorus ammonium of 20 ~ 23%, fully mixes and stirs.
(2) in reactor, adding 330 parts of concentration again is the nitric acid of 65 ~ 68%, reaction 10min.
(3) in reactor, add 105 parts of ammonia neutralizations, the pH controlling material, 6.0, namely obtains the slip of nitrophosphate fertilizer.
(4) slip obtained is dried at 105 DEG C, and pulverizing is powdery nitrophosphate fertilizer, and (total nitrogen content is 26.5%, P
2o
5content is 12%, and wherein nitrate content is 11.7%).
Claims (1)
1. wet phosphoric acid purifying sludge produces a method for polynary nitro-compound fertilizer, it is characterized in that comprising the following steps:
(1) will be 18 ~ 22%P containing massfraction
2o
5phosphoric acid by wet process raffinate, be 20 ~ 23%P containing massfraction
2o
5slag acid and containing massfraction be 20 ~ 23%P
2o
5chemical de-magging slag, be 100 ~ 110 parts, 100 ~ 104 parts and 110 ~ 119 parts by mass fraction respectively and join in reactor, fully mix and stir;
(2) in reactor, add mass fraction be again 300 ~ 350 parts of concentration is the nitric acid of 65 ~ 68%, reaction 5 ~ 10min;
(3) in reactor, then add the ammonia neutralization that mass fraction is 95 ~ 105 parts, the pH of material is controlled between 5.0 ~ 6.5, finally obtains the slip of nitrophosphate fertilizer; Direct for the slip of described nitrophosphate fertilizer spray granulating obtained the nitrophosphate fertilizer of granular high-nitrate state nitrogen content, maybe this slip is directly dried at 100 ~ 105 DEG C, pulverize the nitrophosphate fertilizer obtaining powdery high-nitrate state nitrogen content;
Described slag acid and chemical de-magging slag are the by product of manufacture phosphorus ammonium.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9140325B2 (en) | 2009-03-19 | 2015-09-22 | Fox Factory, Inc. | Methods and apparatus for selective spring pre-load adjustment |
| CN104072209A (en) * | 2014-07-16 | 2014-10-01 | 云南常青树化工有限公司 | Method for preparing nitro compound fertilizer by adopting acid sludge produced in the phosphoric acid manufacturing process |
| CN104261900A (en) * | 2014-09-01 | 2015-01-07 | 云南云天化国际化工有限公司 | Method for producing magnesium ammonium phosphate fertilizer by utilizing phosphoric acid sludge through wet process |
| CN104326771B (en) * | 2014-10-22 | 2016-08-31 | 瓮福（集团）有限责任公司 | A kind of method utilizing phosphorus mine tailing to prepare calcium nitrate fertiliser containing magnesium |
| CN104446673A (en) * | 2014-12-05 | 2015-03-25 | 甘肃瓮福化工有限责任公司 | Method for producing calcium superphosphate by using phosphate rock tailings |
| CN105036816B (en) * | 2015-07-28 | 2019-02-22 | 中化云龙有限公司 | A method of the super nutrient of monoammonium phosphate is adjusted using phosphate ore flotation tailings |
| CN106278390A (en) * | 2016-07-19 | 2017-01-04 | 中化化肥有限公司成都研发中心 | A kind of phosphoric acid by wet process acid sludge comprehensive reutilization method |
| CN107954546A (en) * | 2017-11-24 | 2018-04-24 | 天峨县平昌生态农业有限公司 | A kind of processing method for cultivating family's poultry waster water |
| CN110734304A (en) * | 2018-07-19 | 2020-01-31 | 贵州芭田生态工程有限公司 | Nitrophosphate fertilizer and preparation method thereof |
| CN112624849B (en) * | 2020-12-28 | 2022-04-05 | 瓮福（集团）有限责任公司 | Preparation method of high-solubility nitrogen-phosphorus water-soluble fertilizer |
| CN113277885A (en) * | 2021-06-09 | 2021-08-20 | 四川大学 | Resource utilization method of phosphoric acid residues |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161602A (en) * | 2010-12-28 | 2011-08-24 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium compound fertilizer by utilizing raffinate and phosphate tailings with high magnesium content |
| CN102602904A (en) * | 2012-04-16 | 2012-07-25 | 瓮福（集团）有限责任公司 | Method for producing monoammonium phosphate from raffinate acid |
| CN102924158A (en) * | 2012-12-01 | 2013-02-13 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multielement nitro-compound fertilizer |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161602A (en) * | 2010-12-28 | 2011-08-24 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium compound fertilizer by utilizing raffinate and phosphate tailings with high magnesium content |
| CN102602904A (en) * | 2012-04-16 | 2012-07-25 | 瓮福（集团）有限责任公司 | Method for producing monoammonium phosphate from raffinate acid |
| CN102924158A (en) * | 2012-12-01 | 2013-02-13 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multielement nitro-compound fertilizer |
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Owner name: SINOFERT LIMITED Free format text: FORMER OWNER: CHONGQING PHOSPHATE COMPOUND FERTILIZER ENGINEERING TECHNOLOGY RESEARCH CENTER OF SINOFERT CO., LTD. Effective date: 20150216 |
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