CN108383097A - 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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- CN108383097A CN108383097A CN201810462098.0A CN201810462098A CN108383097A CN 108383097 A CN108383097 A CN 108383097A CN 201810462098 A CN201810462098 A CN 201810462098A CN 108383097 A CN108383097 A CN 108383097A
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- ammonium polyphosphate
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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
- C05B—PHOSPHATIC FERTILISERS
- 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, at 80~110 DEG C, reaction generates monoammonium phosphate, is concentrated by heat filtering, freezing and crystallizing, centrifuges, and 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 sprayed and is neutralized into reactor, white water-soluble ammonium polyphosphate is generated.Ammonium polyphosphate product nitrogen content 15~25% of the present invention, phosphorus pentoxide content 50~65%, N+P2O5Content is more than 76%, and (25 DEG C) of solubility is 25~75g/100g H2O, average degree of polymerization are 5~15, and water-insoluble is less than 0.5%.The production process of the present invention is at low cost, easy to operate, particularly suitable for industrialized production.
Description
Technical field
The invention belongs to fertilizer preparing technical field, specifically a kind of production of agricultural water dissolubility ammonium polyphosphate
Method.
Background technology
Ammonium polyphosphate is a kind of nitrogenous and phosphorus Quadrafos, and wherein nitrogen and phosphorus element content is higher.When polymerization degree n is more 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 using same process route, technological parameter difference is very big.
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 with ammonia in tubular reactor, is generated
Molten state high-concentration polyphosphoric acid ammonium adds water cooling at the liquid fertilizer product of commerical grade 10-34-0 (N P and K mass fraction).
US3342579 is disclosed prepares ammonium polyphosphate with the method for being passed through ammonia in polyphosphoric acid.CN103373717A is disclosed with poly- phosphorus
Acid reacts with ammonium hydrogen carbonate and prepares ammonium polyphosphate in a kettle.
2) 85% orthophosphoric acid carries out condensation with urea and prepares 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 are reacted 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 of preparation
Ammonium phosphate solubility is 18~52g/100gH2O can not produce the liquid fertilizer product of 10-34-0 grades.
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):49-50. novel fertilizer
Expect ammonium polyphosphate production technology and applies pre-test [J] chemical fertilizer industries, 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 carries out condensation with ammonia and prepares 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 are 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 energy consumption can be increased.In addition, to prepare phosphoric acid impurity more for the industrial wet method generally used, water solubility poly is directly prepared with it
Ammonium phosphate, it is difficult to obtain the white ammonium polyphosphate product of high-dissolvability.In the technique for preparing ammonium polyphosphate with phosphoric acid, phosphoric acid
It is easy to etching apparatus, 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.
Invention content
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 prepare water-soluble ammonium polyphosphate 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 is：
A method of using extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate, include the following steps：
(1) ammonia is continuously passed through in the reactor containing extraction phosphoric acid by wet process, in 80~110 DEG C of reactions, reaction terminates
Reaction solution is subjected to heat filtering concentration, freezing and crystallizing, centrifugation successively 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 sprayed carries out neutralization reaction into atomization reactor and ammonia, generates
Spherical ammonium polyphosphate；Spherical ammonium polyphosphate obtains the water-soluble ammonium polyphosphate of white powder after pulverizing.
Step (1) is specially：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 passes through heat filtering concentration, freezing and crystallizing, centrifugation successively, 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 mechanically；Mother liquor and three times mother liquor are discharged after merging, and are given birth into using other methods
In the system for producing industrial grade monoammonium phosphate.
In step (1), it is in liquefied ammonia, triethylamine, monoethanolamine, ethylenediamine to wash the lye used in monoammonium phosphate crude product
It is at least one.
Extract a concentration of the 20~85% of phosphoric acid by wet process.
Step (2) is specially：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, condensation reaction 10~30 minutes, and obtained acid ammonium polyphosphate melt is 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) is specially：Atomization reactor is heated to 150~250 DEG C, ammonia is passed through instead by atomization by compressor
It answers in device, it is 0.1~3MPa to make ammonia partial pressure in atomization reactor；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 more than 76%, and (25 DEG C) of solubility is 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 advantageous effect is：
1. primary raw material used by the production method of the present 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 the production method of the present invention is extraction phosphoric acid by wet process first produces monoammonium phosphate with ammonia, 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 directly to apply (solid nitrogen content
15~25%, solid phosphorus content 50~65%), can also be applied at the composite fertilizer of various proportionings as Raw material processing
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.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Specific implementation mode
Technical scheme of the present invention is further described below by way of specific embodiment, but protection scope of the present invention
It is not limited to these examples.Every protection model that the present 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% contents, it is anti-at 110 DEG C
Monoammonium phosphate should be generated, the reaction time is 120 minutes, and reaction solution is obtained by heat filtering concentration, freezing and crystallizing, centrifugation
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 mechanically, a mother liquor and
Mother liquor merges discharge three times, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure 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% contents extraction phosphoric acid by wet process, is reacted at 80 DEG C
Monoammonium phosphate is generated, the reaction time is 60 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, and a mother liquor and three times mother liquor close
And be discharged, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 0.1MPa in atomization reactor, then urinates liquid acid ammonium polyphosphate melt and 5kg foaming agents
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% contents extraction phosphoric acid by wet process, is reacted at 100 DEG C
Monoammonium phosphate is generated, the reaction time is 100 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, a mother liquor and three times mother
Liquid merges discharge, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 0.1MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 250kg foaming agents
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% contents extraction phosphoric acid by wet process, is reacted at 110 DEG C
Monoammonium phosphate is generated, the reaction time is 60 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, and a mother liquor and three times mother liquor merge row
Go out, into the system for producing industrial grade monoammonium phosphate using 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,
Ensure that ammonia partial pressure is 0.5MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 55kg foaming agents 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% contents extraction phosphoric acid by wet process, is reacted at 90 DEG C
Monoammonium phosphate is generated, the reaction time is 100 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, a mother liquor and three times mother
Liquid merges discharge, into the system for producing industrial grade monoammonium phosphate using other methods.
(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 method
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,
Ensure that ammonia partial pressure is 2MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 1Kg foaming agent azos
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% contents extraction phosphoric acid by wet process, life is reacted at 80 DEG C
At monoammonium phosphate, the reaction time is 120 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, and a mother liquor and three times mother liquor close
And be discharged, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 0.5MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 87Kg foaming agents
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% contents 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 centrifuges, it is thick to obtain monoammonium phosphate
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 mechanically, and a mother liquor and three times mother liquor close
And be discharged, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure 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 from atomization reactor penetrating suitable for reading in reactor, 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% contents extraction phosphoric acid by wet process, life is reacted at 90 DEG C
At monoammonium phosphate, the reaction time is 90 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, and a mother liquor and three times mother liquor merge discharge,
Into in the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 2MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 4kg foaming agent azos
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% contents extraction phosphoric acid by wet process, is reacted at 110 DEG C
Monoammonium phosphate is generated, the reaction time is 120 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, a mother liquor and three times mother
Liquid merges discharge, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 0.8MPa in atomization reactor, it is then that liquid acid ammonium polyphosphate melt and 56Kg foaming agents is empty
Gas, with ammonia neutralization reaction 50 minutes, gives birth to glomerate ammonium polyphosphate 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 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% contents extraction phosphoric acid by wet process, life is reacted at 80 DEG C
At monoammonium phosphate, the reaction time is 120 minutes, is concentrated by heat filtering, freezing and crystallizing, centrifuges, 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 mechanically, and a mother liquor and three times mother liquor close
And be discharged, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 0.1MPa in atomization reactor, then urinates liquid acid ammonium polyphosphate melt and 56Kg foaming agents
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% contents 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 centrifuges, it is thick to obtain monoammonium phosphate
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 mechanically, a mother liquor and three times mother liquor
Merge discharge, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure 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 penetrating atomization reactor suitable for reading, and with ammonia neutralization reaction 35 minutes, life was 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% contents extraction phosphoric acid by wet process, life is reacted at 95 DEG C
At monoammonium phosphate, the reaction time is 120 minutes, and through overheat filter concentration, freezing and crystallizing centrifuges, 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 mechanically.Mother liquor and three times
Mother liquor merges discharge, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 1.5MPa in atomization reactor, then urinates liquid acid ammonium polyphosphate melt and 60Kg foaming agents
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% contents 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 centrifuges, 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 mechanically, and a mother liquor and three times mother liquor merge discharge, is entered
In the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 0.15MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 165kg foaming agents
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% contents extraction phosphoric acid by wet process, life is reacted at 90 DEG C
At monoammonium phosphate, the reaction time is 110 minutes, and through overheat filter concentration, freezing and crystallizing centrifuges, 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 mechanically, and a mother liquor and three times mother liquor close
And be discharged, into the system for producing industrial grade monoammonium phosphate using other methods.
(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,
Ensure that ammonia partial pressure is 0.13MPa in atomization reactor, then by liquid acid ammonium polyphosphate melt and 35Kg foaming agents
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, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is 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 is characterized in that include the following steps：
(1) ammonia is continuously passed through in the reactor containing extraction phosphoric acid by wet process, in 80~110 DEG C of reactions, after reaction will
Reaction solution carries out heat filtering concentration, freezing and crystallizing, centrifugation successively, 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 continuously spray and carry out neutralization reaction into atomization reactor and ammonia, 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) is specially：Ammonia is continuously passed through containing extraction wet method
In the reactor of phosphoric acid, reacted 60~120 minutes at 80~110 DEG C, reaction solution successively pass through heat filtering concentration, freezing and crystallizing,
It centrifuges, 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 mechanically；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), it is liquid to wash the lye used in monoammonium phosphate crude product
At least one of ammonia, triethylamine, monoethanolamine, ethylenediamine.
4. according to the method for claims 1 or 2, it is characterised in that：Extract a concentration of the 20~85% of phosphoric acid by wet process.
5. the method according to claim 1, it is characterised in that：Step (2) is specially：Fixed bed reactors are heated to 200~
350 DEG C, monoammonium phosphate salt crystal is continuously added to from the suitable for reading of fixed bed reactors, condensation reaction 10~30 minutes obtains
Acid ammonium polyphosphate melt is flowed out from the lower mouth of fixed bed reactors；By-product water steam is waved from the suitable for reading of fixed bed reactors
It sends out, the water steam containing ammonia is passed through to the reaction for carrying out step (1) in the reactor containing extraction phosphoric acid by wet process.
6. the method according to claim 1, it is characterised in that：Step (3) is specially：Atomization reactor is heated to 150~250
DEG C, ammonia is passed through in atomization reactor by compressor, it is 0.1~3MPa to make ammonia partial pressure in atomization reactor；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 being 1~60:100.
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