CN101456759B - Method for producing magnesium ammonium phosphate composite fertilizer - Google Patents
Method for producing magnesium ammonium phosphate composite fertilizer Download PDFInfo
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- CN101456759B CN101456759B CN 200810197992 CN200810197992A CN101456759B CN 101456759 B CN101456759 B CN 101456759B CN 200810197992 CN200810197992 CN 200810197992 CN 200810197992 A CN200810197992 A CN 200810197992A CN 101456759 B CN101456759 B CN 101456759B
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- magnesium
- ammonium phosphate
- phosphorus
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- composite fertilizer
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Abstract
The invention relates to a method for producing an ammonium magnesium phosphate compound fertilizer, which comprises: taking phosphorus-magnesium waste residue generated during wet-method phosphoric acid refining as a raw material, and adding a small amount of compounds containing Mg<2+> to make up for the deficiency of magnesium in the waste residue; adding ammonia water, taking an alkaline solution as an acidity regulator, and performing mixing and stirring reaction at room temperature, wherein the reaction time is not less than 60 minutes, the stoichiometric mol ratio of the Mg<2+> to NH4<+> to PO4<3-> in the mixed reaction liquid is 1-1.2:1:1, and the pH value of the reaction liquid is controlled to be between 8.0 and 10.0; and performing solid-liquid separation, wherein solid material is the ammonium magnesium phosphate compound fertilizer containing phosphorus, ammonia and magnesium. By adoption of the method to prepare the ammonium magnesium phosphate compound fertilizer, the economic benefit can be increased; the wet-method phosphoric acid refining cost can be reduced; resource waste can be prevented; and the economic benefit can be improved.
Description
Technical field
The present invention relates to a kind of production method of the magnesium ammonium phosphate composite fertilizer of producing by the waste residue behind the wet phosphoric acid refining.
Background technology
Magnesium ammonium phosphate is a kind of nitrogenous (N5.5%), phosphorus (P
2O
527.5%), the multi-elements composite fertilizer of magnesium (Mg0.15%), and all the components is all effective, solubleness is extremely low in water, owing to have solubility in citric acid, so after using, can store nitrogen in soil.Starting late in domestic research and production aspect for magnesium ammonium phosphate, up to the present, does not see the industrialization report.Since the eighties in 20th century, many universities and scientific research institution are studied the technology of producing magnesium ammonium phosphate.Area, Langfang, Hebei province chemical institute is with the filtration of bicarbonate mother liquor and produce magnesium ammonium phosphate by phosphoric acid extraction in the general calcium; East China Li Ding university develops wet method and produces the MgNH4PO4 novel process; The multiple fertile institute of Zhengzhou University's phosphorus is to MgNH
4PO
4Reaction system carried out phase balance determining, but magnesium ammonium phosphate composite fertilizer does not all have large-scale production.
Summary of the invention
Purpose of the present invention is exactly that will to provide a kind of be the production method of the magnesium ammonium phosphate composite fertilizer of raw material production with a large amount of waste residues that produce in the wet phosphoric acid refining.This method technical process is short, and equipment is simple, is convenient to operation, is easy to realize suitability for industrialized production.
The object of the present invention is achieved like this: a kind of production method of magnesium ammonium phosphate composite fertilizer is a raw material with the phosphorus magnesium waste residue that produces in the wet phosphoric acid refining process, is contained Mg on a small quantity
2+The compound deficiency of replenishing magnesium in the waste residue, add ammoniacal liquor again, as acidity regulator, at room temperature mix stirring reaction with basic solution, the reaction times is no less than 60 minutes, the Mg in the mixed reaction solution
2+, NH
4 +, PO
4 3-The stoichiometry mol ratio be Mg
2+: NH
4 +: PO
4 3-=1～1.2: 1: 1, the pH value of reaction solution was controlled between the 8.0-10.0, carried out solid-liquid separation then, and solid matter is the ammonium phosphate fertiliser containing magnesium that contains phosphorus, ammonia, magnesium.
The phosphorus magnesium waste residue that produces behind the wet phosphoric acid refining is meant and contains phosphorus pentoxide content 10-30%, contains magnesium 3%-15%, the solid slag of pH value 3-7.
Describedly add a spot of Mg of containing
2+Compound be meant wherein one or more of magnesium oxide or magnesium hydroxide or magnesiumcarbonate.
Described acidity regulator is wherein one or more of sodium hydroxide or ammoniacal liquor or magnesiumcarbonate or magnesium oxide.
In the wet phosphoric acid refining process, can produce a large amount of slags that contains phosphorus magnesium, whenever refining 1 ton of phosphoric acid by wet process, expense slag about 3 tons is probably arranged, these slags are handled through method of the present invention and are made magnesium ammonium phosphate composite fertilizer, can increase economic benefit, reduce the wet phosphoric acid refining cost, prevent the wasting of resources, increase economic efficiency.
Embodiment
Specific implementation process of the present invention is as follows:
Contain phosphorus pentoxide content 10-30% with what produce in the wet phosphoric acid refining process, contain magnesium 3%-15%, the pH value is contained Mg on a small quantity for the phosphorus magnesium waste residue of 3-7 is a raw material
2+The compound deficiency of replenishing magnesium in the waste residue, add ammoniacal liquor again, as acidity regulator, at room temperature mix stirring reaction with basic solution, the reaction times is no less than 60 minutes, the Mg in the mixed reaction solution
2+, NH
4 +, PO
4 3-The stoichiometry mol ratio be Mg
2+: NH
4 +: PO
4 3-=1～1.2: 1: 1, the pH value of reaction solution was controlled between the 8.0-10.0, carried out solid-liquid separation then, and solid matter is the magnesium ammonium phosphate composite fertilizer that contains phosphorus, ammonia, magnesium.
Describedly add a spot of Mg of containing
2+Compound be meant wherein one or more of magnesium oxide or magnesium hydroxide or magnesiumcarbonate.
Described acidity regulator is wherein one or more of sodium hydroxide or ammoniacal liquor or magnesiumcarbonate or magnesium oxide.
The slag of the reaction deliming that produces behind the wet phosphoric acid refining is decided to be 1
#Slag, content are Vanadium Pentoxide in FLAKES 10%, Mg content 5%; Slag after the neutralization reaction is decided to be 2
#Slag, content are Vanadium Pentoxide in FLAKES 27%, Mg content 10%.
Embodiment 1:
Get 1
#Slag 100g adds an amount of water, at room temperature, and according to stoichiometric ratio Mg
2+: PO4
3-: NH4
+=1～1.2: 1: 1 condition, be docile and obedient preface again and add magnesium oxide and ammoniacal liquor, regulate control pH value of solution value 8.0～10.0 with sodium hydroxide, reaction is no less than 60 minutes, after reaction finishes, carry out solid-liquid separation, solid is exactly the magnesium ammonium phosphate product, wherein nitrogenous 5.2%, magnesium oxide 15.1%, Vanadium Pentoxide in FLAKES 28.5%, and the utilization ratio of phosphorus is 93% in the slag, the utilization ratio of magnesium is 97%, and filtrate water is returned and added recycle in the raw material slag again.
Embodiment 2:
Get 1
#Slag 100g adds an amount of water, at room temperature, and according to stoichiometric ratio Mg
2+: PO4
3-: NH4
+=1～1.2: 1: 1 condition, be docile and obedient preface again and add magnesium hydroxide and ammoniacal liquor, regulate control pH value of solution value 8.0～10.0 with ammoniacal liquor, reaction is no less than 60 minutes, after reaction finishes, carry out solid-liquid separation, solid is exactly the magnesium ammonium phosphate product, wherein nitrogenous 5.1%, magnesium oxide 15.3%, Vanadium Pentoxide in FLAKES 28.4%, and the utilization ratio of phosphorus is 94% in the slag, the utilization ratio of magnesium is 97%, and filtrate water is returned and added recycle in the raw material slag again.
Embodiment 3:
Get 1
#Slag 100g adds an amount of water, at room temperature, and according to stoichiometric ratio Mg
2+: PO4
3-: NH4
+=1～1.2: 1: 1 condition, be docile and obedient preface again and add magnesiumcarbonate and ammoniacal liquor, regulate control pH value of solution value 8.0～10.0 with magnesiumcarbonate, reaction is no less than 60 minutes, after reaction finishes, carry out solid-liquid separation, solid is exactly the magnesium ammonium phosphate product, wherein nitrogenous 5.2%, magnesium oxide 15.0%, Vanadium Pentoxide in FLAKES 28.8%, and the utilization ratio of phosphorus is 94% in the slag, the utilization ratio of magnesium is 97%, and filtrate water is returned and added recycle in the raw material slag again.
Embodiment 4:
Get 2
#Slag 100g adds an amount of water, at room temperature, and according to stoichiometric ratio Mg
2+: PO4
3-: NH4
+=1～1.2: 1: 1 condition, be docile and obedient preface again and add magnesium oxide and ammoniacal liquor, regulate control pH value of solution value 8.0～10.0 with magnesium oxide, reaction is no less than 60 minutes, after reaction finishes, carry out solid-liquid separation, solid is exactly the magnesium ammonium phosphate product, wherein nitrogenous 5.6%, magnesium oxide 15.5%, Vanadium Pentoxide in FLAKES 29.2%, and the utilization ratio of phosphorus is 95% in the slag, the utilization ratio of magnesium is 98%, and filtrate water is returned and added recycle in the raw material slag again.
Embodiment 5:
Get 2
#Slag 100g adds an amount of water, at room temperature, and according to stoichiometric ratio Mg
2+: PO4
3-: NH4
+=1～1.2: 1: 1 condition, be docile and obedient preface again and add magnesium hydroxide and ammoniacal liquor, regulate control pH value of solution value 8.0～10.0 with sodium hydroxide, magnesiumcarbonate and magnesium oxide, reaction is no less than 60 minutes, after reaction finishes, carry out solid-liquid separation, solid is exactly the magnesium ammonium phosphate product, wherein nitrogenous 5.5%, magnesium oxide 15.5%, Vanadium Pentoxide in FLAKES 29.7%, and the utilization ratio of phosphorus is 94% in the slag, the utilization ratio of magnesium is 98%, and filtrate water is returned and added recycle in the raw material slag again.
Embodiment 6:
Get 2
#Slag 100g adds an amount of water, at room temperature, and according to stoichiometric ratio Mg
2+: PO4
3-: NH4
+=1～1.2: 1: 1 condition, be docile and obedient preface again and add magnesiumcarbonate and ammoniacal liquor, regulate control pH value of solution value 8.0～10.0 with sodium hydroxide, ammoniacal liquor and magnesiumcarbonate, reaction is no less than 60 minutes, after reaction finishes, carry out solid-liquid separation, solid is exactly the magnesium ammonium phosphate product, wherein nitrogenous 5.4%, magnesium oxide 15.1%, Vanadium Pentoxide in FLAKES 29.4%, and the utilization ratio of phosphorus is 95% in the slag, the utilization ratio of magnesium is 98%, and filtrate water is returned and added recycle in the raw material slag again.
Claims (2)
1. the production method of a magnesium ammonium phosphate composite fertilizer is characterized in that: with the phosphorus magnesium waste residue that produces in the wet phosphoric acid refining process is raw material, is contained Mg on a small quantity
2+The compound deficiency of replenishing magnesium in the waste residue, add ammoniacal liquor again, as acidity regulator, at room temperature mix stirring reaction with basic solution, the reaction times is no less than 60 minutes, the Mg in the mixed reaction solution
2+, NH
4 +, PO
4 3-The stoichiometry mol ratio be Mg
2+: NH
4 +: PO
4 3-=1～1.2: 1: 1, the pH value of reaction solution was controlled between the 8.0-10.0, carried out solid-liquid separation then, and solid matter is the magnesium ammonium phosphate composite fertilizer that contains phosphorus, ammonia, magnesium, the described Mg that contains
2+Compound be meant wherein one or more of magnesium oxide or magnesium hydroxide or magnesiumcarbonate, described acidity regulator is wherein one or more of sodium hydroxide or ammoniacal liquor or magnesiumcarbonate or magnesium oxide.
2. the production method of a kind of magnesium ammonium phosphate composite fertilizer according to claim 1, it is characterized in that: the phosphorus magnesium waste residue that produces behind the wet phosphoric acid refining is meant and contains phosphorus pentoxide content 10-30%, contains magnesium 3%-15%, the solid slag of pH value 3-7.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810197992 CN101456759B (en) | 2008-11-28 | 2008-11-28 | Method for producing magnesium ammonium phosphate composite fertilizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810197992 CN101456759B (en) | 2008-11-28 | 2008-11-28 | Method for producing magnesium ammonium phosphate composite fertilizer |
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|---|---|
| CN101456759A CN101456759A (en) | 2009-06-17 |
| CN101456759B true CN101456759B (en) | 2010-08-18 |
Family
ID=40767917
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|---|---|---|---|
| CN 200810197992 Active CN101456759B (en) | 2008-11-28 | 2008-11-28 | Method for producing magnesium ammonium phosphate composite fertilizer |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102923684A (en) * | 2012-11-09 | 2013-02-13 | 瓮福（集团）有限责任公司 | Method for utilizing magnesium bicarbonate aqueous solution to produce magnesium ammonium phosphate compound fertilizer |
| CN102924158B (en) * | 2012-12-01 | 2014-03-05 | 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 |
| CN103936489B (en) * | 2014-04-29 | 2015-12-30 | 昆明隆祥化工有限公司 | A kind of method of producing magnesium ammonium phosphate slow release fertilizer |
| CN105293459B (en) * | 2014-06-04 | 2017-08-18 | 深圳市芭田生态工程股份有限公司 | The method of the complete water-soluble MAP of Wet-process Phosphoric Acid Production and coproduction ammonium magnesium phosphate |
| 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 |
| CN105439646A (en) * | 2015-08-26 | 2016-03-30 | 云南三环中化化肥有限公司 | Method for producing phosphorus magnesia fertilizer by using wet phosphoric acid residues |
| 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 |
| CN106745109A (en) * | 2016-11-29 | 2017-05-31 | 长沙秋点兵信息科技有限公司 | Acid leaching process refines the processing method of waste liquid produced by cobalt nickel |
| CN108996791B (en) * | 2018-08-03 | 2021-02-12 | 山东和生海洋科技有限公司 | Novel process for seawater desalination and comprehensive utilization |
| CN112174699A (en) * | 2020-09-07 | 2021-01-05 | 昆明隆祥化工有限公司 | Method for producing magnesium ammonium phosphate slow-release fertilizer by wet-process phosphoric acid |
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