CN108383097B - A method of utilizing extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate - Google Patents
A method of utilizing extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate Download PDFInfo
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- CN108383097B CN108383097B CN201810462098.0A CN201810462098A CN108383097B CN 108383097 B CN108383097 B CN 108383097B CN 201810462098 A CN201810462098 A CN 201810462098A CN 108383097 B CN108383097 B CN 108383097B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
- C01B25/405—Polyphosphates of ammonium
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
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- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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Abstract
The invention discloses a kind of methods using extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate.First ammonia is continuously passed through in extraction wet-process phosphoric acid reaction device, generates monoammonium phosphate in 80~110 DEG C of reactions, be concentrated, freezing and crystallizing, be centrifugated by heat filtering, alkali liquid washing obtains monoammonium phosphate crystal；Monoammonium phosphate salt is added continuously in fixed bed reactors again, in 200~350 DEG C of melt condensations at acid ammonium polyphosphate；Finally under the conditions of atomization temperature of reactor is 150~250 DEG C, ammonia partial pressure is 0.1~3MPa, the mixture of acid ammonium polyphosphate melt and foaming agent is continuously neutralized into reactor by spraying, generates white water-soluble ammonium polyphosphate.Ammonium polyphosphate product nitrogen content 15~25% of the present invention, phosphorus pentoxide content 50~65%, N+P2O5Content is greater than 76%, and (25 DEG C) of solubility are 25~75g/100g H2O, average degree of polymerization are 5~15, and water-insoluble is less than 0.5%.Production process of the invention is at low cost, easy to operate, particularly suitable for industrialized production.
Description
Technical field
The invention belongs to fertilizer preparation technical field, specifically a kind of production of agricultural water dissolubility ammonium polyphosphate
Method.
Background technique
Ammonium polyphosphate is a kind of nitrogenous and phosphorus Quadrafos, and wherein nitrogen and phosphorus element content is higher.When polymerization degree n is greater than
It is insoluble in water, commonly referred to as high ammonium polyphosphate when 20, is industrial widely applied fire retardant；When polymerization degree n is 2~20,
Commonly referred to as water-soluble ammonium polyphosphate, is the important source material of liquid fertilizer.In addition, water-soluble ammonium polyphosphate chemical property is steady
Fixed, for pH close to neutrality, dissolubility is good；And it is high containing nitrogen and phosphorus element needed for plant, there is stronger chelation to metal ion,
It can be used for making liquid composite fertilizer, and can gradually hydrolyze, be absorbed and utilized well by plant, it is long to can be used as a kind of slow dissolubility
Imitate fertilizer.
Ammonium polyphosphate synthesis route according to the literature, mainly have wet phosphoric acid, phosphoric acid and urea condensation method,
Polyphosphoric acid ammoniation process and ammonium orthophosphate dehydration polymerization method, these methods in the technique for preparing high ammonium polyphosphate by wide coverage,
And the production method report of water-soluble ammonium polyphosphate is relatively fewer.
Water-soluble ammonium polyphosphate is due to the difference of product average degree of polymerization, and the difference shown in terms of application performance is very
Greatly；Even if technological parameter difference is very big using same process route.
1) polyphosphoric acids is first prepared, and then prepares water-soluble ammonium polyphosphate.
US3382059 is disclosed with commodity wet-process phosphoric acid concentration into peroxophosphoric acid, is reacted in tubular reactor with ammonia, is generated
Molten state high-concentration polyphosphoric acid ammonium adds water to be cooled to the liquid fertilizer product of commerical grade 10-34-0 (N P and K mass fraction).
US3342579, which is disclosed, prepares ammonium polyphosphate with the method for being passed through ammonia in polyphosphoric acid.CN103373717A is disclosed with poly- phosphorus
Acid reacts in a kettle with ammonium hydrogen carbonate and prepares ammonium polyphosphate.
2) 85% orthophosphoric acid and urea carry out condensation and prepare water-soluble ammonium polyphosphate
CN103787726A discloses a kind of ammonium polyphosphate water soluble fertilizer and preparation method thereof, this method by phosphoric acid,
Urea, potassium sulfate, zinc chloride, copper chloride, borax and auxiliary material are added to reaction kettle and react 30~45 minutes at 180~185 DEG C, then
It is warming up to 200~205 DEG C of reactions, 1.5~2 hours obtained ammonium polyphosphates.The preparation method is simple, practical, but the poly prepared
Ammonium phosphate solubility is 18~52g/100gH2O can not produce the liquid fertilizer product of 10-34-0 grade.
If preparing water-soluble ammonium polyphosphate using low concentration phosphoric acid, need be at content by the Phosphoric Acid Concentration of low concentration
85% phosphoric acid (preparation and application [J] the phosphate fertilizer and compound fertilizer of agricultural ammonium polyphosphate, 2008,23 (2): the novel fertilizer of 49-50.
Expect ammonium polyphosphate production technology and apply pre-test [J] chemical fertilizer industry, 2008,35 (4): 16-17. industry ammonium polyphosphate it is simple
It is printed when preparing chemical industry, 1999, (11): 34-35).
3) 85% orthophosphoric acid and ammonia carry out condensation and prepare water-soluble ammonium polyphosphate
In current production of phosphate fertilizer, ammonia is generally passed through with low concentration phosphoric acid and is prepared into monoammonium phosphate.For monoammonium phosphate
Water-soluble ammonium polyphosphate is prepared for primary raw material, is required to that various condensing agents (Archie V.US3264087A is added；Hahn
H..US4104362A；The bright .CN104528682A. of woods).
If dehydration equipment need to be increased, not only increases cost at 50% even higher content the Phosphoric Acid Concentration of low content,
And it will increase energy consumption.In addition, to prepare phosphoric acid impurity more for the wet process industrially generallyd use, water-soluble poly is directly prepared with it
Ammonium phosphate, it is difficult to obtain the white ammonium polyphosphate product of high-dissolvability.It is prepared in the technique of ammonium polyphosphate with phosphoric acid, phosphoric acid
It is easy to corrode equipment, reactor material is required high.Urea, which easily decomposes, generates a large amount of ammonias and carbon dioxide gas, makes to polymerize
A large amount of foams are formed in journey causes flash.
Therefore, it is badly in need of a kind of production method for the water-soluble ammonium polyphosphate that production cost is low, solubility is high.
Summary of the invention
The present invention provides a kind of method using extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate, first produces phosphoric acid one
Ammonium salt, then water-soluble ammonium polyphosphate is prepared by raw material of monoammonium phosphate salt, foaming agent and ammonia.This method has production cost
It is low, it is easy to operate, the advantages that particularly suitable for industrialized production；The white water-soluble ammonium polyphosphate solubility of production is high, directly
Or the excellent water soluble fertilizer of processability as raw material.
The technical solution adopted by the present invention are as follows:
A method of utilizing extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate, comprising the following steps:
(1) ammonia is continuously passed through in the reactor containing extraction phosphoric acid by wet process, is reacted in 80~110 DEG C, reaction terminates
Reaction solution is successively subjected to heat filtering concentration, freezing and crystallizing, centrifuge separation afterwards, obtains monoammonium phosphate crystal；
(2) monoammonium phosphate crystal continuous is added in fixed bed reactors, it is more at acid in 200~350 DEG C of melt condensations
Ammonium polyphosphate melt；
(3) under conditions of atomization temperature of reactor is 150~250 DEG C, ammonia partial pressure is 0.1~3MPa, by step (2)
Obtained acid ammonium polyphosphate melt and foaming agent is continuously spraying to enter atomization reactor and ammonia progress neutralization reaction, generates
Spherical ammonium polyphosphate；Spherical ammonium polyphosphate obtains the water-soluble ammonium polyphosphate of white powder after pulverizing.
Step (1) specifically: ammonia is continuously passed through in the reactor containing extraction phosphoric acid by wet process, it is anti-at 80~110 DEG C
It answers 60~120 minutes, reaction solution successively passes through heat filtering concentration, freezing and crystallizing, centrifuge separation, obtains monoammonium phosphate crude product and one
Secondary mother liquor；By monoammonium phosphate crude product alkali liquid washing, monoammonium phosphate crystal and secondary mother liquid are obtained；Lye warp in secondary mother liquid
Recovery processing obtains mother liquor three times, and lye is applied；Mother liquor and three times mother liquor are discharged after merging, raw into utilization other methods
In the system for producing industrial grade monoammonium phosphate.
In step (1), lye used in monoammonium phosphate crude product is washed as in liquefied ammonia, triethylamine, monoethanolamine, ethylenediamine
It is at least one.
The concentration for extracting phosphoric acid by wet process is 20~85%.
Step (2) specifically: fixed bed reactors are heated to 200~350 DEG C, by monoammonium phosphate salt crystal from fixed bed
The suitable for reading of reactor is continuously added to, and condensation reaction 10~30 minutes, obtained acid ammonium polyphosphate melt was from fixed bed reaction
The lower mouth of device flows out；By-product water steam is volatilized from the suitable for reading of fixed bed reactors, and the water steam containing ammonia is passed through and is contained
There is the reaction that step (1) is carried out in the reactor of extraction phosphoric acid by wet process.
Step (3) specifically: atomization reactor is heated to 150~250 DEG C, ammonia is passed through instead by atomization by compressor
It answers in device, making to be atomized ammonia partial pressure in reactor is 0.1~3MPa；Acid ammonium polyphosphate melt that step (2) is obtained and
The mixture of foaming agent is from the penetrating suitable for reading of atomization reactor, and in fresh ammonia and 30~60 minutes glomerate poly phosphorus of life
Sour ammonium is pulverized spherical ammonium polyphosphate with idler wheel, is squeezed out from the lower mouth of atomization reactor, is obtained the water-soluble of white powder
Property ammonium polyphosphate.
In step (3), the foaming agent is oxamides, urea, aminoquinoxaline, ammonium hydrogen carbonate, azodiisobutyronitrile, sky
Gas, CO2、N2At least one of.
In step (3), the mass ratio of foaming agent and monoammonium phosphate is 1~60:100.
Water solubility ammonium polyphosphate product nitrogen content 15~25% of the invention, phosphorus pentoxide content 50~65%, N+P2O5
Content is greater than 76%, and (25 DEG C) of solubility are 25~75g/100gH2O, average degree of polymerization are 5~15, and water-insoluble is less than
0.5%.
Compared with prior art, the present invention beneficial effect is:
1. primary raw material used by production method of the invention is extraction phosphoric acid by wet process, compared with prior art primary raw material
Using orthophosphoric acid, polyphosphoric acid, phosphorus pentoxide, have that raw material is cheap and easy to get, impurity is few in monoammonium phosphate, production cost
Low, the advantages that equipment investment is few, the reaction time is short.
2. technique used by production method of the invention is that extraction phosphoric acid by wet process and ammonia first produce monoammonium phosphate, compare
The prior art, monoammonium phosphate salt are small to equipment corrosion, compared to wet phosphoric acid, orthophosphoric acid urea condensation method, polyphosphoric acid ammonification
Method etc., the present invention have the characteristics that process conditions are simple.
3. water solubility ammonium polyphosphate produced by the invention can be used as solid composite fertilizer material and directly apply (solid nitrogen content
15~25%, solid phosphorus content 50~65%), can also be applied as Raw material processing at the compound fertilizer of various proportions
With.Or be configured to liquid fertilizer, especially high-concentration liquid fertilizer (liquid nitrogen content 10~15%, liquid phosphorus content 30~
40%) it is administered, prepared fertilizer application mode, which includes that base manure, top dressing, foliage-spray, root dipping or seed manure are same, to be broadcast.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Hereinafter, the technical scheme of the present invention will be further described by specific examples, but protection scope of the present invention
It is not limited to these examples.It is all that protection model of the invention is included in without departing substantially from the change of present inventive concept or equivalent substitute
Within enclosing.
Embodiment 1
(1) ammonia is continuously passed through in the reactor for the extraction phosphoric acid by wet process for being equipped with 2000Kg20% content, it is anti-at 110 DEG C
Monoammonium phosphate should be generated, the reaction time is 120 minutes, and reaction solution passes through heat filtering concentration, freezing and crystallizing, centrifuge separation, obtains
Monoammonium phosphate crude product and a mother liquor；Monoammonium phosphate crude product triethylamine alkali liquid washing, obtains 400kg monoammonium phosphate crystal and two
Secondary mother liquor；The recovered processing of triethylamine lye in secondary mother liquid obtains mother liquor three times, and triethylamine lye is applied, a mother liquor and
Mother liquor merges discharge three times, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 350 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 150 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.1MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 4kg foaming agent ammonia
The mixture of base ammonium formate is raw with fresh ammonia neutralization reaction 30 minutes from atomization reactor penetrating atomization reactor suitable for reading
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, is obtained white by glomerate ammonium polyphosphate
Color powdery, water-soluble ammonium polyphosphate product 380kg.Product index is shown in Table 1.
Embodiment 2
(1) ammonia is continuously passed through in the reactor for being equipped with 1000Kg50% content extraction phosphoric acid by wet process, is reacted at 80 DEG C
Monoammonium phosphate is generated, the reaction time is 60 minutes, is concentrated, freezing and crystallizing by heat filtering, is centrifugated, it is thick to obtain monoammonium phosphate
Product and a mother liquor；Monoammonium phosphate crude product monoethanolamine alkali liquid washing, obtains 500kg monoammonium phosphate crystal and secondary mother liquid；
The recovered processing of lye in secondary mother liquid obtains mother liquor three times, and monoethanolamine lye is applied, and a mother liquor and three times mother liquor close
And be discharged, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 200 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 250 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.1MPa in atomization reactor, then urinates liquid acid ammonium polyphosphate melt and 5kg foaming agent
The mixture of element, with fresh ammonia neutralization reaction 60 minutes, generates spherical from atomization reactor penetrating atomization reactor suitable for reading
Ammonium polyphosphate, by idler wheel by spherical ammonium polyphosphate product from atomization reactor under mouth squeeze out, obtain white powder
The water-soluble ammonium polyphosphate product 475kg of shape.Product index is shown in Table 1.
Embodiment 3
(1) ammonia is continuously passed through in the reactor for being equipped with 500Kg85% content extraction phosphoric acid by wet process, is reacted at 100 DEG C
Monoammonium phosphate is generated, the reaction time is 100 minutes, is concentrated, freezing and crystallizing by heat filtering, is centrifugated, obtains monoammonium phosphate
Crude product and a mother liquor；Monoammonium phosphate crude product ethylenediamine alkali liquid washing, obtains 415kg monoammonium phosphate crystal and secondary mother liquid；
The recovered processing of ethylenediamine lye in secondary mother liquid obtains mother liquor three times, and ethylenediamine lye is applied, a mother liquor and three times mother
Liquid merges discharge, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 250 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 10
Minute.
(3) atomization reactor is first heated to 200 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.1MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 250kg foaming agent
The mixture of oxamides, with fresh ammonia neutralization reaction 30 minutes, is generated from atomization reactor penetrating atomization reactor suitable for reading
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, obtains white by spherical ammonium polyphosphate
Powdery, water-soluble ammonium polyphosphate product 395kg.Product index is shown in Table 1.
Embodiment 4
(1) ammonia is continuously passed through in the reactor for being equipped with 1000Kg55% content extraction phosphoric acid by wet process, is reacted at 110 DEG C
Monoammonium phosphate is generated, the reaction time is 60 minutes, is concentrated, freezing and crystallizing by heat filtering, is centrifugated, it is thick to obtain monoammonium phosphate
Product and a mother liquor；Monoammonium phosphate crude product liquefied ammonia alkali liquid washing, obtains 550kg monoammonium phosphate crystal and secondary mother liquid；It is secondary
The recovered processing of liquefied ammonia lye in mother liquor obtains mother liquor three times, and liquefied ammonia lye is applied, and a mother liquor and three times mother liquor merge row
Out, in the system for producing industrial grade monoammonium phosphate into utilization other methods.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 265 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 200 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.5MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 55kg foaming agent N2
From atomization reactor penetrating atomization reactor suitable for reading, with fresh ammonia neutralization reaction 60 minutes, raw glomerate polyphosphoric acids
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, obtains the water solubility of white powder by ammonium
Ammonium polyphosphate product 522kg.Product index is shown in Table 1.
Embodiment 5
(1) ammonia is continuously passed through in the reactor for being equipped with 1000Kg28% content extraction phosphoric acid by wet process, is reacted at 90 DEG C
Monoammonium phosphate is generated, the reaction time is 100 minutes, is concentrated, freezing and crystallizing by heat filtering, is centrifugated, obtains monoammonium phosphate
Crude product and a mother liquor；Monoammonium phosphate crude product triethylamine alkali liquid washing, obtains 280kg monoammonium phosphate crystal and secondary mother liquid；
The recovered processing of triethylamine lye in secondary mother liquid obtains mother liquor three times, and triethylamine lye is applied, a mother liquor and three times mother
Liquid merges discharge, into the system using other methods production industrial grade monoammonium phosphate.
(2) heating device is opened, the temperature of fixed bed reactors is risen to and is maintained at 200-350 DEG C, by ammonium hydrogen phosphate
Salt is continuously added to from fixed bed reactors are suitable for reading, and melt condensation is condensed the water of generation at liquid acid ammonium polyphosphate melt
Steam from fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction wet process
In phosphoric acid and monoammonium phosphate is generated, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time
It is 30 minutes.
(3) atomization reactor is first heated to 250 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 2MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 1Kg foaming agent azo
The mixture of bis-isobutyronitrile is raw with fresh ammonia neutralization reaction 30 minutes from atomization reactor penetrating atomization reactor suitable for reading
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, is obtained white by glomerate ammonium polyphosphate
Color powdery, water-soluble ammonium polyphosphate product 266kg.Product index is shown in Table 1.
Embodiment 6
(1) ammonia is continuously passed through in the reactor for being equipped with 600Kg48% content extraction phosphoric acid by wet process, is given birth in 80 DEG C of reactions
At monoammonium phosphate, the reaction time is 120 minutes, is concentrated by heat filtering, freezing and crystallizing, is centrifugated, it is thick to obtain monoammonium phosphate
Product and a mother liquor；Monoammonium phosphate crude product monoethanolamine alkali liquid washing, obtains 288kg monoammonium phosphate crystal and secondary mother liquid；
The recovered processing of lye in secondary mother liquid obtains mother liquor three times, and monoethanolamine lye is applied, and a mother liquor and three times mother liquor close
And be discharged, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 300 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 180 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.5MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 87Kg foaming agent
CO2Gas is from atomization reactor penetrating atomization reactor suitable for reading, and with fresh ammonia neutralization reaction 60 minutes, life was glomerate more
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, it is more to obtain white water-soluble by ammonium polyphosphate
Ammonium polyphosphate product 274kg.Product index is shown in Table 1.
Embodiment 7
(1) ammonia is continuously passed through in the reactor for being equipped with 400Kg85% content extraction phosphoric acid by wet process, is reacted at 110 DEG C
Monoammonium phosphate is generated, the reaction time is 120 minutes, and through overheat filter concentration, freezing and crystallizing, it is thick to obtain monoammonium phosphate for centrifuge separation
Product and a mother liquor；Monoammonium phosphate crude product monoethanolamine alkali liquid washing, obtains 340kg monoammonium phosphate crystal and secondary mother liquid；
The recovered processing of lye in secondary mother liquid obtains mother liquor three times, and monoethanolamine lye is applied, and a mother liquor and three times mother liquor close
And be discharged, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 350 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 10
Minute.
(3) atomization reactor is first heated to 250 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.1MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 34Kg foaming agent carbon
The mixture of sour hydrogen ammonium is atomized in reactor from atomization reactor penetrating suitable for reading, with fresh ammonia neutralization reaction 60 minutes, is generated
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, obtains white by spherical ammonium polyphosphate
Powdery, water-soluble ammonium polyphosphate product 290kg.Product index is shown in Table 1.
Embodiment 8
(1) ammonia is continuously passed through in the reactor for being equipped with 800Kg50% content extraction phosphoric acid by wet process, is given birth in 90 DEG C of reactions
At monoammonium phosphate, the reaction time is 90 minutes, is concentrated by heat filtering, freezing and crystallizing, is centrifugated, obtains monoammonium phosphate crude product
With a mother liquor；Monoammonium phosphate crude product liquefied ammonia alkali liquid washing, obtains 400kg monoammonium phosphate crystal and secondary mother liquid；Secondary mother
The recovered processing of liquefied ammonia lye in liquid obtains mother liquor three times, and liquefied ammonia lye is applied, and a mother liquor and three times mother liquor merge discharge,
Into in the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 260 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 180 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 2MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 4kg foaming agent azo
The mixture of bis-isobutyronitrile is raw with fresh ammonia neutralization reaction 60 minutes from atomization reactor penetrating atomization reactor suitable for reading
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, is obtained white by glomerate ammonium polyphosphate
Color powdery, water-soluble ammonium polyphosphate product 380kg.Product index is shown in Table 1.
Embodiment 9
(1) ammonia is continuously passed through in the reactor for being equipped with 1000Kg28% content extraction phosphoric acid by wet process, is reacted at 110 DEG C
Monoammonium phosphate is generated, the reaction time is 120 minutes, is concentrated, freezing and crystallizing by heat filtering, is centrifugated, obtains monoammonium phosphate
Crude product and a mother liquor；Monoammonium phosphate crude product ethylenediamine alkali liquid washing, obtains 280kg monoammonium phosphate crystal and secondary mother liquid；
The recovered processing of ethylenediamine lye in secondary mother liquid obtains mother liquor three times, and ethylenediamine lye is applied, a mother liquor and three times mother
Liquid merges discharge, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 300 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 250 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.8MPa in atomization reactor, it is then that liquid acid ammonium polyphosphate melt and 56Kg foaming agent is empty
Gas is from atomization reactor penetratings suitable for reading atomization reactor, and ammonia neutralization reaction 50 minutes, gives birth to glomerate ammonium polyphosphate,
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, obtains the water-soluble poly of white powder
Ammonium phosphate product 265kg.Product index is shown in Table 1.
Embodiment 10
(1) ammonia is continuously passed through in the reactor for being equipped with 800Kg45% content extraction phosphoric acid by wet process, is given birth in 80 DEG C of reactions
At monoammonium phosphate, the reaction time is 120 minutes, is concentrated by heat filtering, freezing and crystallizing, is centrifugated, it is thick to obtain monoammonium phosphate
Product and a mother liquor；Monoammonium phosphate crude product monoethanolamine alkali liquid washing, obtains 360kg monoammonium phosphate crystal and secondary mother liquid；
The recovered processing of lye in secondary mother liquid obtains mother liquor three times, and monoethanolamine lye is applied, and a mother liquor and three times mother liquor close
And be discharged, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 320 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 15
Minute.
(3) atomization reactor is first heated to 220 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.1MPa in atomization reactor, then urinates liquid acid ammonium polyphosphate melt and 56Kg foaming agent
The mixture of element, with fresh ammonia neutralization reaction 60 minutes, generates spherical from atomization reactor penetrating atomization reactor suitable for reading
Ammonium polyphosphate, by idler wheel by spherical ammonium polyphosphate product from atomization reactor under mouth squeeze out, obtain white powder
The water-soluble ammonium polyphosphate product 310kg of shape.Product index is shown in Table 1.
Embodiment 11
(1) ammonia is continuously passed through in the reactor for being equipped with 1000Kg48% content extraction phosphoric acid by wet process, is reacted at 90 DEG C
Monoammonium phosphate is generated, the reaction time is 100 minutes, and through overheat filter concentration, freezing and crystallizing, it is thick to obtain monoammonium phosphate for centrifuge separation
Product and a mother liquor；Monoammonium phosphate crude product ethylenediamine alkali liquid washing, obtains 480kg monoammonium phosphate crystal and secondary mother liquid；Two
The recovered processing of ethylenediamine lye in secondary mother liquor obtains mother liquor three times, and ethylenediamine lye is applied, a mother liquor and three times mother liquor
Merge discharge, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 240 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 250 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.1MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 4.8Kg foaming urine
The mixture of element is from atomization reactor penetratings suitable for reading atomization reactor, and ammonia neutralization reaction 35 minutes, gives birth to glomerate more
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, obtains white powder by ammonium polyphosphate
Water-soluble ammonium polyphosphate product 455kg.Product index is shown in Table 1.
Embodiment 12
(1) ammonia is continuously passed through in the reactor for being equipped with 500Kg60% content extraction phosphoric acid by wet process, is given birth in 95 DEG C of reactions
At monoammonium phosphate, the reaction time is 120 minutes, and through overheat filter concentration, freezing and crystallizing, centrifuge separation obtains monoammonium phosphate crude product
With a mother liquor.Monoammonium phosphate crude product monoethanolamine alkali liquid washing, obtains 300kg monoammonium phosphate crystal and secondary mother liquid.Two
The recovered processing of monoethanolamine lye in secondary mother liquor obtains mother liquor three times, and monoethanolamine lye is applied.Mother liquor and three times
Mother liquor merges discharge, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 280 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 180 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 1.5MPa in atomization reactor, then urinates liquid acid ammonium polyphosphate melt and 60Kg foaming agent
The mixture of element, with fresh ammonia neutralization reaction 60 minutes, generates spherical from atomization reactor penetrating atomization reactor suitable for reading
Ammonium polyphosphate, by idler wheel by spherical ammonium polyphosphate product from atomization reactor under mouth squeeze out, obtain white powder
The water-soluble ammonium polyphosphate product 285kg of shape.Product index is shown in Table 1.
Embodiment 13
(1) ammonia is continuously passed through in the reactor for being equipped with 600Kg55% content extraction phosphoric acid by wet process, is reacted at 100 DEG C
Monoammonium phosphate is generated, the reaction time is 70 minutes, and through overheat filter concentration, freezing and crystallizing, centrifuge separation obtains monoammonium phosphate crude product
With a mother liquor；Monoammonium phosphate crude product liquefied ammonia alkali liquid washing, obtains 330kg monoammonium phosphate crystal and secondary mother liquid；Secondary mother
The recovered processing of lye in liquid obtains mother liquor three times, and liquefied ammonia lye is applied, and a mother liquor and three times mother liquor merge discharge, is entered
In system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 240 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 160 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.15MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 165kg foaming agent
Ammonium hydrogen carbonate is from atomization reactor penetrating atomization reactor suitable for reading, and with fresh ammonia neutralization reaction 40 minutes, life was glomerate
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, obtains white water-soluble by ammonium polyphosphate
Ammonium polyphosphate product 315kg.Product index is shown in Table 1.
Embodiment 14
(1) ammonia is continuously passed through in the reactor for being equipped with 500Kg70% content extraction phosphoric acid by wet process, is given birth in 90 DEG C of reactions
At monoammonium phosphate, the reaction time is 110 minutes, and through overheat filter concentration, freezing and crystallizing, centrifuge separation obtains monoammonium phosphate crude product
With a mother liquor；Monoammonium phosphate crude product triethylamine alkali liquid washing, obtains 350kg monoammonium phosphate crystal and secondary mother liquid；It is secondary
The recovered processing of triethylamine lye in mother liquor obtains mother liquor three times, and triethylamine lye is applied, and a mother liquor and three times mother liquor close
And be discharged, into the system using other methods production industrial grade monoammonium phosphate.
(2) open heating device, the temperature of fixed bed reactors is risen to and be maintained at 290 DEG C, by ammonium hydrogen phosphate salt from
Fixed bed reactors are suitable for reading to be continuously added to, and melt condensation is condensed the vapor of generation at liquid acid ammonium polyphosphate melt
From fixed bed reactors volatilization suitable for reading, the vapor containing ammonia enter containing extraction phosphoric acid by wet process reactor in extraction phosphoric acid by wet process
It neutralizes and generates monoammonium phosphate, liquid acid ammonium polyphosphate melt mouth under fixed bed reactors flows out, the reaction time 30
Minute.
(3) atomization reactor is first heated to 160 DEG C, then fresh ammonia is passed through in atomization reactor by compressor,
Guarantee that ammonia partial pressure is 0.13MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 35Kg foaming agent
Ammonium hydrogen carbonate is from atomization reactor penetrating atomization reactor suitable for reading, and with fresh ammonia neutralization reaction 45 minutes, life was glomerate
Spherical ammonium polyphosphate product is squeezed out from mouth under atomization reactor by idler wheel, obtains white water-soluble by ammonium polyphosphate
Ammonium polyphosphate product 120kg.Product index is shown in Table 1.
1 embodiment of table, 1~18 nutrient content transitivity parameter list
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of method using extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate, which comprises the following steps:
(1) ammonia is continuously passed through in the reactor containing extraction phosphoric acid by wet process, is reacted in 80~110 DEG C, after reaction will
Reaction solution successively carries out heat filtering concentration, freezing and crystallizing, centrifuge separation, obtains monoammonium phosphate crystal；
(2) monoammonium phosphate crystal continuous is added in fixed bed reactors, in 200~350 DEG C of melt condensations at acid poly phosphorus
Sour ammonium melt；
(3) under conditions of atomization temperature of reactor is 150~250 DEG C, ammonia partial pressure is 0.1~3MPa, step (2) is obtained
Acid ammonium polyphosphate melt and foaming agent is continuously spraying enters atomization reactor and ammonia carries out neutralization reaction, generate spherical
Ammonium polyphosphate；Spherical ammonium polyphosphate obtains the water-soluble ammonium polyphosphate of white powder after pulverizing.
2. the method according to claim 1, it is characterised in that: step (1) specifically: be continuously passed through ammonia containing extraction wet process
In the reactor of phosphoric acid, 80~110 DEG C react 60~120 minutes, reaction solution successively pass through heat filtering concentration, freezing and crystallizing,
Centrifuge separation, obtains monoammonium phosphate crude product and a mother liquor；By monoammonium phosphate crude product alkali liquid washing, monoammonium phosphate crystal is obtained
And secondary mother liquid；The recovered processing of lye in secondary mother liquid obtains mother liquor three times, and lye is applied；Mother liquor and three times mother liquor
It is discharged after merging.
3. method according to claim 2, it is characterised in that: in step (1), washing lye used in monoammonium phosphate crude product is liquid
At least one of ammonia, triethylamine, monoethanolamine, ethylenediamine.
4. method according to claim 1 or 2, it is characterised in that: the concentration for extracting phosphoric acid by wet process is 20~85wt%.
5. the method according to claim 1, it is characterised in that: step (2) specifically: fixed bed reactors are heated to 200~
350 DEG C, monoammonium phosphate crystal is continuously added to from the suitable for reading of fixed bed reactors, condensation reaction 10~30 minutes, obtained acid
Formula ammonium polyphosphate melt is flowed out from the lower mouth of fixed bed reactors；Suitable for reading volatilization of the by-product water steam from fixed bed reactors
Out, the water steam containing ammonia is passed through to the reaction that step (1) is carried out in the reactor containing extraction phosphoric acid by wet process.
6. the method according to claim 1, it is characterised in that: step (3) specifically: atomization reactor is heated to 150~250
DEG C, ammonia is passed through in atomization reactor by compressor, making to be atomized ammonia partial pressure in reactor is 0.1~3MPa；By step
(2) mixture of the acid ammonium polyphosphate melt and foaming agent that obtain is from the penetrating suitable for reading for being atomized reactor, with fresh ammonia
30~60 minutes glomerate ammonium polyphosphates of life are neutralized, are pulverized spherical ammonium polyphosphate with idler wheel, from atomization reactor
Lower mouth squeeze out, obtain the water-soluble ammonium polyphosphate of white powder.
7. method according to claim 1 or 6, it is characterised in that: in step (3), the foaming agent is oxamides, urine
Element, aminoquinoxaline, ammonium hydrogen carbonate, azodiisobutyronitrile, air, CO2、N2At least one of.
8. method according to claim 1 or 6, it is characterised in that: in step (3), the quality of foaming agent and monoammonium phosphate
Than for 1~60:100.
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