CN103113139A - 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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- CN103113139A CN103113139A CN2013100696511A CN201310069651A CN103113139A CN 103113139 A CN103113139 A CN 103113139A CN 2013100696511 A CN2013100696511 A CN 2013100696511A CN 201310069651 A CN201310069651 A CN 201310069651A CN 103113139 A CN103113139 A CN 103113139A
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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 is produced polynary nitro-compound fertilizer.
Background technology
After phosphoric acid by wet process is purified with extraction agent, remaining acid is called as raffinate, and its main component is 18～22% P
2O
5, and a large amount of impurity.Along with the consumption of high-quality phosphate rock resource, the 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 on August 24th, 2011 disclosed Chinese patent CN102161602A, relate to and a kind ofly prepare the method for phosphorus magnesium compound fertilizer as raw material take wet phosphoric acid purifying by-product raffinate and high magnesium phosphor tail slag, although this method can be processed raffinate, P in its raffinate used
2O
5Content is 42～46%, processes raffinate with this method and belongs to waste to phosphor resource, does not promote its due value.
Utilize phosphoric acid what slag to produce the flow process of powdery monoammonium phosphate in prior art, the quick ammonification neutralization of employing pump circulation, two-effect evaporation concentrate, drying process with atomizing, dilute phosphoric acid [design: w(P
2O
5) 24%～26%, w(is solid) 4%～6%] in the quick ammoniation reactor of pump circulation with gas ammonia reaction, and constantly circulation neutralization in endless tube outside; Slip after neutralization first by II effect, I effect evaporation concentration, is then sent into drying tower through high-pressure pump, advances the quantity of steam of I effect well heater by control and controls into the water content of drying tower slip, slip w(H
2O) be controlled at 22%～25%; Send into the slip of drying tower through high-pressure pump after the pressure nozzle atomizing, be dried in the time of from top to bottom with the hot gas flow counter current contact, the qualified powdery finished product that generates after the hot gas flow drying.But this flow process is oversize, and has two step concentration processs to make energy consumption and cost increase.
Nowadays also can produce a large amount of chemical slags in the industrial ammonium phosphate production process, but its P
2O
5Content is between 20～23%.If it is not processed, not only can cause the pollution of environment, but also can cause the waste of resource.
The shortcoming of prior art: the method for existing processing raffinate and phosphoric acid sludge all 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 a kind of method that technique is simple, energy consumption is low, cost is low and the costly wet phosphoric acid purifying sludge of products obtained therefrom is produced polynary nitro-compound fertilizer.
The present invention seeks to realize like this: a kind of wet phosphoric acid purifying sludge is produced the method for polynary nitro-compound fertilizer, and its key is to comprise the following steps:
(1) will contain massfraction is 18～22%P
2O
5The phosphoric acid by wet process raffinate, to contain massfraction be 20～23%P
2O
5Slag acid and to contain 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) adding mass fraction in the reactor again is that 300～350 parts of concentration are 65～68% nitric acid, reaction 5～10min;
(3) then adding mass fraction in the reactor is the ammonia neutralization of 95～105 parts, and the pH of material is controlled between 5.0～6.5, obtains at last the slip of nitrophosphate fertilizer.
The direct spray granulating of the slip of above-mentioned nitrophosphate fertilizer is obtained the nitrophosphate fertilizer of granular high-nitrate state nitrogen content, maybe this slip is directly dried, pulverized the nitrophosphate fertilizer that obtains powdery high-nitrate state nitrogen content under 100～105 ℃.
Above-mentioned slag acid and chemical de-magging slag are the by product of manufacture phosphorus ammonium.
Beneficial effect:
The method that a kind of wet phosphoric acid purifying sludge of the present invention is produced 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 wet phosphoric acid purifying and the waste material of industrial production phosphorus ammonium fully can be reused, turn waste into wealth, obtain costly product, save the energy, reduced widely industrial pollution.
Embodiment
Embodiment 1:
A kind of wet phosphoric acid purifying sludge is produced the method for polynary nitro-compound fertilizer, comprises the following steps:
(1) adding 100 parts to reactor, to contain massfraction be 18～22%P
2O
5Phosphoric acid by wet process raffinate, 100 parts to contain massfraction be 20～23%P
2O
5The slag acid of manufacture phosphorus ammonium and 119 parts to contain massfraction be 20～23%P
2O
5The chemical de-magging slag of manufacture phosphorus ammonium, fully mix and stir.
(2) adding 350 parts of concentration in the reactor is 65～68% nitric acid again, reaction 10min.
(3) add 105 parts of ammonia neutralizations in reactor, control the pH of material 5.0, namely obtained the slip of nitrophosphate fertilizer.
(4) the direct spray granulating of resulting slip just can obtain the nitrophosphate fertilizer of granular high-nitrate state nitrogen content (total nitrogen content is 26%, P
2O
5Content is 12%, and wherein nitrate content is 12%).
Embodiment 2:
A kind of wet phosphoric acid purifying sludge is produced the method for polynary nitro-compound fertilizer, comprises the following steps:
(1) adding 107 parts to reactor, to contain massfraction be 18～22%P
2O
5Phosphoric acid by wet process raffinate, 104 parts to contain massfraction be 20～23%P
2O
5The slag acid of manufacture phosphorus ammonium and 110 parts to contain massfraction be 20～23%P
2O
5The chemical de-magging slag of manufacture phosphorus ammonium, fully mix and stir.
(2) adding 300 parts of concentration in the reactor is 65～68% nitric acid again, reaction 10min.
(3) add 95 parts of ammonia neutralizations in reactor, control the pH of material 5.0, namely obtained the slip of nitrophosphate fertilizer.
(4) the direct spray granulating of resulting slip just can obtain the nitrophosphate fertilizer of granular high-nitrate state nitrogen content (total nitrogen content is 25%, P
2O
5Content is 13.5%, and wherein nitrate content is 11%).
Embodiment 3:
A kind of wet phosphoric acid purifying sludge is produced the method for polynary nitro-compound fertilizer, comprises the following steps:
(1) add 105 parts of P to reactor
2O
5Massfraction is 18～22% phosphoric acid by wet process raffinate, 104 parts of P
2O
5Massfraction is slag acid and 112 parts of P of 20～23% manufacture phosphorus ammonium
2O
5Massfraction is the chemical de-magging slag of 20～23% manufacture phosphorus ammonium, fully mixes and stirs.
(2) adding 300 parts of concentration in the reactor is 65～68% nitric acid again, reaction 10min.
(3) add 105 parts of ammonia neutralizations in reactor, control the pH of material 6.5, namely obtained the slip of nitrophosphate fertilizer.
(4) resulting slip is dried under 100 ℃, 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:
A kind of wet phosphoric acid purifying sludge is produced the method for polynary nitro-compound fertilizer, comprises the following steps:
(1) add 102 parts of P to reactor
2O
5Massfraction is 18～22% phosphoric acid by wet process raffinate, 100 parts of P
2O
5Massfraction is slag acid and 118 parts of P of 20～23% manufacture phosphorus ammonium
2O
5Massfraction is the chemical de-magging slag of 20～23% manufacture phosphorus ammonium, fully mixes and stirs.
(2) adding 330 parts of concentration in the reactor is 65～68% nitric acid again, reaction 10min.
(3) add 105 parts of ammonia neutralizations in reactor, control the pH of material 6.0, namely obtained the slip of nitrophosphate fertilizer.
(4) resulting slip is dried under 105 ℃, 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 (3)
1. a wet phosphoric acid purifying sludge is produced the method for polynary nitro-compound fertilizer, it is characterized in that comprising the following steps:
(1) will contain massfraction is 18～22%P
2O
5The phosphoric acid by wet process raffinate, to contain massfraction be 20～23%P
2O
5Slag acid and to contain 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) adding mass fraction in the reactor again is that 300～350 parts of concentration are 65～68% nitric acid, reaction 5～10min;
(3) then adding mass fraction in the reactor is the ammonia neutralization of 95～105 parts, and the pH of material is controlled between 5.0～6.5, obtains at last the slip of nitrophosphate fertilizer.
2. a kind of wet phosphoric acid purifying sludge method of producing polynary nitro-compound fertilizer according to claim 1, it is characterized in that: the direct spray granulating of the slip of described nitrophosphate fertilizer is obtained the nitrophosphate fertilizer of granular high-nitrate state nitrogen content, maybe this slip is directly dried, pulverized the nitrophosphate fertilizer that obtains powdery high-nitrate state nitrogen content under 100～105 ℃.
3. a kind of wet phosphoric acid purifying sludge method of producing polynary nitro-compound fertilizer according to claim 1, it is characterized in that: described slag acid and chemical de-magging slag are the by product of manufacture phosphorus ammonium.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104326771A (en) * | 2014-10-22 | 2015-02-04 | 瓮福（集团）有限责任公司 | Method for preparing calcium-magnesium nitrate fertilizer by utilizing phosphate tailings |
| 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 |
| CN105036816A (en) * | 2015-07-28 | 2015-11-11 | 中化化肥有限公司成都研发中心 | Method for adjusting enriched nutrients in monoammonium phosphate through utilizing phosphate 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 |
| CN112624849A (en) * | 2020-12-28 | 2021-04-09 | 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 |
| US12103349B2 (en) | 2009-03-19 | 2024-10-01 | Fox Factory, Inc. | Methods and apparatus for selective spring pre-load adjustment |
Citations (3)
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| 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 |
-
2013
- 2013-03-05 CN CN201310069651.1A patent/CN103113139B/en active Active
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 |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US12103349B2 (en) | 2009-03-19 | 2024-10-01 | 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 |
| CN104326771A (en) * | 2014-10-22 | 2015-02-04 | 瓮福（集团）有限责任公司 | Method for preparing calcium-magnesium nitrate fertilizer by utilizing phosphate tailings |
| 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 |
| CN105036816A (en) * | 2015-07-28 | 2015-11-11 | 中化化肥有限公司成都研发中心 | Method for adjusting enriched nutrients in monoammonium phosphate through utilizing phosphate 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 |
| CN112624849A (en) * | 2020-12-28 | 2021-04-09 | 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 |
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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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