CN108218513A - A kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability - Google Patents

A kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability Download PDF

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Publication number
CN108218513A
CN108218513A CN201810226423.3A CN201810226423A CN108218513A CN 108218513 A CN108218513 A CN 108218513A CN 201810226423 A CN201810226423 A CN 201810226423A CN 108218513 A CN108218513 A CN 108218513A
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fertilizer
nitrogen
preparation
phosphorus
storage stability
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CN201810226423.3A
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CN108218513B (en
Inventor
吴舒
王金铭
杨振军
梁红江
洪伟
茹铁军
王金刚
贲艳英
肖占梅
何栋
任宇红
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SINO-ARAB CHEMICAL FERTILIZER Co Ltd
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SINO-ARAB CHEMICAL FERTILIZER Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
    • C05G5/00Fertilisers characterised by their form
    • C05G5/10Solid or semi-solid fertilisers, e.g. powders
    • C05G5/12Granules or flakes
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B11/00Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
    • C05B11/04Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
    • C05B11/06Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using nitric acid (nitrophosphates)

Abstract

The invention discloses a kind of preparation methods of the granular nitro high-nitrogen compound fertilizer with high storage stability, belong to chemical fertilizer preparing technical field, its step are as follows:(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus;(2) preparation of solid material;(3) preparation of granule materials;(4) preparation of the granular nitro high-nitrogen compound fertilizer with high storage stability:By granule materials obtained by step (3) by drying, screening, cooling, package process, the granular nitro high-nitrogen compound fertilizer with high storage stability is obtained.The present invention improves the storage stability of particle nitro-compound fertilizer material by optimization of C/C composites and technique, and significant effect is easy to carry out.

Description

A kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability
Technical field
It is more particularly to a kind of with high storage stability the present invention relates to a kind of preparation method of nitro high-nitrogen compound fertilizer The preparation method of granular nitro high-nitrogen compound fertilizer, belongs to chemical fertilizer preparing technical field.
Background technology
Compound fertilizer mainly includes ammonium nitrogen, amidonitrogen and nitrate nitrogen, wherein nitrate nitrogen for the nitrogen source that crop provides It is a kind of quick-acting nitrogen sources needed for plant, is that quick-acting compound fertilizers and water soluble fertilizer must be to be added.Nitrogen is by nitrate anion (NO3 -1) and ammonium root (NH4 +1) composition is known as nitro-compound fertilizer, the industrial crops such as tobacco, fruit tree, most vegetables are hobby nitre states Nitrogen, particularly with some crops to nitrate nitrogen sensitivity, the ratio of nitrate nitrogen and ammonium nitrogen influences whether crop in fertilizer Yield.
Nitro high-nitrogen compound fertilizer (refers to N P and K total nutrient more than 40%, wherein total nitrogen content ≤17%, and nitrate nitrogen Account for more than 28% total nitrogen) structure is very unstable in storing process is stacked, fertilizer is easily hardened into bulk, lose flowability and Dispersibility, can not spread fertilizer over the fields or mechanized application, many inconvenience be caused to user, so granulated fertilizer is steady during storage Qualitative is an important index.
The source of nitrate nitrogen is mainly provided using ammonium nitrate phosphorus (ANP) in conventional compound fertilizer formula, especially right In nitro high-nitrogen compound fertilizer, the dosage of ammonium nitrate phosphorus (ANP) in formula is up to 30-40%, and ammonium nitrate phosphorus (ANP) refers to industrial nitre Sour ammonium (AN) carries out uprising modified obtained agricultural fertilizer, and due to having, good water solubility, quick-acting, nitrogen content is high, of low cost The advantages that, agriculturally very popular.In general, ammonium nitrate (AN) solution is with powdery monoammonium phosphate, uprising dose on a small quantity, according to certain Ratio congruent melting (ammonium nitrate (AN) that mass fraction is 90% or so and the monoammonium phosphate that mass fraction is 10% or so) whitewashing is made Grain obtains prilled ammonium nitrate phosphorus (ANP).Phosphorus element, uprising dose of introducing ammonium nitrate (AN), modified purpose are to improve anti-knock properties, are added in Ammonium nitrate phosphorus (ANP) after modifying agent can not be reduced into ammonium nitrate (AN), and not explosibility, the safety of ammonium nitrate phosphorus (ANP) Can more it stablize, therefore, ammonium nitrate phosphorus (ANP) becomes the raw material of composite heat transfer instead of ammonium nitrate (AN).Ammonium nitrate phosphorus (ANP) nutrient content is 32-4 or so (nitrogenous 32%, containing phosphorus pentoxide 4%).Fertilizer industry is to ammonium nitrate phosphorus (ANP) Focus is typically nutrient content, nitrate nitrogen content, anti-knock properties, thermal stability, high temperature safety, and for ammonium nitrate phosphorus (ANP) Physical property and structural analysis in terms of report it is also less.
Existing preventing blocking technology is the coating anticaking agent of outer surface more, makes to be physically isolated between fertiliser granulates, reach To the purpose for slowing down caking, such as using inert powder, high molecular polymer, surfactant, organic hydrophobing agent etc..But It is at present, anti-caking to be coated with by surface, effect basically reaches maximization, continues to be coated with anticaking agent, Neng Gouti from outer surface The anti-caking limitation risen, and universal due to industrialized agriculture, to the physical property of fertilizer there has also been tightened up requirement, therefore Reduce the introducing of water-insoluble and oil product can avoid fertilizer result in blockage to drip irrigation facilities caused by economic loss.
Therefore it provides a kind of storage stability that can further improve granular nitro high-nitrogen compound fertilizer and reducing water The introducing of insoluble matter and oil product and then the granular nitro with high storage stability that fertilizer is avoided to result in blockage drip irrigation facilities The preparation method of high-nitrogen compound fertilizer just becomes the technical field and is badly in need of the technical barrier solved.
Invention content
The object of the present invention is to the problem of storage for nitro high-nitrogen compound fertilizer is unstable, provides one kind and is deposited with height The preparation method of the granular nitro high-nitrogen compound fertilizer of stability is stored up, granulated fertilizer is made to be protected during prolonged packed stacking It is fixed to keep steady, youngster prevented from caking.
The above-mentioned purpose of the present invention reaches by the following technical programs:
Scheme 1:
A kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 10%-34%, the potassium nitrate of 9%-30%, by which part are accounted for Potassium nitrate forms common solution with ammonium nitrate phosphorus, the constant temperature at 90-135 DEG C, and stirring is dried, cooled down and crushes, and forms modified nitre state Nitrogen;
(2) preparation of solid material
By in the modification nitrate nitrogen obtained in step (1), remaining potassium nitrate and fertilizer formula other ammonium nitrogen sources, phosphorus Source, sylvite, filler are stirred, and mixed material is transported in rotary drum granulator by feed belt, obtains solid material;
(3) preparation of granule materials
The liquid nitrogen for accounting for fertilizer gross mass 4.3%-4.5% (is accounted for fertilizer gross mass, provided by liquefied ammonia, similarly hereinafter), accounts for fertilizer The phosphorus pentoxide (account for fertilizer gross mass, provided by phosphoric acid, similarly hereinafter) of gross mass 6.78%-6.84% is provided, accounts for fertilizer gross mass The sulfate radical (being provided by sulfuric acid, similarly hereinafter) of 9.6%-10.22%, after being sufficiently mixed in tubular reactor, obtains liquid phase material, Be ejected into the solid material of step (2), in tubular reactor simultaneously be passed through cleaning solution for adjust granulation humidity, liquid phase Material is coated with granulating particle with solid-phase material in rotary drum granulator;Liquid phase feed passes through the Flux Valve Control unit interval Addition;Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is made for adjusting Grain humidity, obtains granule materials;
(4) preparation of the granular nitro high-nitrogen compound fertilizer with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, obtain that there is high storage stability Granular nitro high-nitrogen compound fertilizer.
Preferably, in the step (1), the part potassium nitrate accounts for 2 weight %-35 weight % of ammonium nitrate phosphorus.
Preferably, in the step (1), the modified nitrate nitrogen is powder, and powder granularity is below 40 mesh.
Preferably, in the step (1), mass percent of the ammonium nitrate phosphorus (ANP) in fertilizer formula is 13.1%- 31.27%, the mass percent of potassium nitrate is 9.56%-28.67%.
Scheme 2:
A kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability, its step are as follows:
(1) melt process of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 10%-34%, the potassium nitrate of 9%-30%, by which part are accounted for Potassium nitrate is with ammonium nitrate phosphorus by high-temperature fusion, and after forming slurry, whitewashing curing, cooling forms modified nitrate nitrogen;
(2) preparation of solid material
By in the modification nitrate nitrogen obtained in step (1), remaining potassium nitrate and fertilizer formula other ammonium nitrogen sources, phosphorus Source, sylvite, filler are stirred, and mixed material is transported in rotary drum granulator by feed belt, obtains solid material;
(3) preparation of granule materials
The liquid nitrogen of fertilizer gross mass 4.3%-4.5% will be accounted for, account for five oxidations two of fertilizer gross mass 6.78%-6.84% Phosphorus accounts for the sulfate radical of fertilizer gross mass 9.6%-10.22%, after being sufficiently mixed in tubular reactor, obtains liquid phase material, spray Be mapped in the solid material of step (2), in tubular reactor simultaneously be passed through cleaning solution for adjust granulation humidity, liquid phase object Material is coated with granulating particle with solid-phase material in rotary drum granulator;Liquid phase feed is added by the Flux Valve Control unit interval Enter amount;Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is granulated for adjusting Humidity obtains granule materials;
(4) preparation of the granular nitro high-nitrogen compound fertilizer with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, obtain that there is high storage stability Granular nitro high-nitrogen compound fertilizer.
Preferably, in the step (1), the part potassium nitrate accounts for 1 weight %-10 weight % of ammonium nitrate phosphorus.
Preferably, in the step (1), the modified nitrate nitrogen is granular, the particle of below average grain diameter 2.8mm.
Preferably, in the step (1), mass percent of the ammonium nitrate phosphorus (ANP) in fertilizer formula is 13.1%- 31.27%, the mass percent of potassium nitrate is 9.56%-28.67%.
Scheme 3:
A kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 10%-34%, the potassium nitrate of 9%-30%, by which part are accounted for Potassium nitrate forms common solution with ammonium nitrate phosphorus, the constant temperature at 90-135 DEG C, and stirring forms stable common solution, spare;
(2) preparation of solid material
By in remaining potassium nitrate in step (1) and fertilizer formula other ammonium nitrogen sources, phosphorus source, sylvite, filler stir Mixing, mixed material are transported to by feed belt in rotary drum granulator, obtain original solid material;It will be obtained in step (1) Common solution be ejected on original solid material by nozzle, participate in bond granulating, obtain solid material;
(3) preparation of granule materials
The liquid nitrogen for accounting for fertilizer gross mass 4.3%-4.5% (is accounted for fertilizer gross mass, provided by liquefied ammonia, similarly hereinafter), accounts for fertilizer The phosphorus pentoxide (account for fertilizer gross mass, provided by phosphoric acid, similarly hereinafter) of gross mass 6.78%-6.84% is provided, accounts for fertilizer gross mass The sulfate radical (being provided by sulfuric acid, similarly hereinafter) of 9.6%-10.22%, after being sufficiently mixed in tubular reactor, obtains liquid phase material, Be ejected into the solid material of step (2), in tubular reactor simultaneously be passed through cleaning solution for adjust granulation humidity, liquid phase Material is coated with granulating particle with solid-phase material in rotary drum granulator;Liquid phase feed passes through the Flux Valve Control unit interval Addition;Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is made for adjusting Grain humidity, obtains granule materials;
(4) preparation of the granular nitro high-nitrogen compound fertilizer with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, obtain that there is high storage stability Granular nitro high-nitrogen compound fertilizer.
Preferably, part potassium nitrate described in the step (1) accounts for 2 weight %-35 weight % of ammonium nitrate phosphorus.
Preferably, in the step (1), the modified nitrate nitrogen is powdery, and powder granularity is below 40 mesh.
Preferably, mass percent of the ammonium nitrate phosphorus (ANP) in fertilizer formula is 13.1%- in the step (1) 31.27%, the mass percent of potassium nitrate is 9.56%-28.67%.
Preferably, the granular nitro high-nitrogen compound fertilizer refers to N P and K total nutrient more than 40%, and wherein nitrogen content exists ≤ 17%, and nitrate nitrogen accounts for more than the 28% of total nitrogen, nitro-compound fertilizer particle size is in 2.0-4.8mm.
Preferably, the grade of the granular nitro high-nitrogen compound fertilizer includes 22-8-10,20-10-10,17-17- 17,18-9-18, but it is not limited to above-mentioned grade.
Preferably, other ammonium nitrogen sources described in the step (2), phosphorus source, sylvite, filler include liquefied ammonia, phosphoric acid, sulphur Acid, potassium sulfate, potassium chloride, ammonium sulfate, monoammonium phosphate, calcium superphosphate and sepiolite.
Preferably, other ammonium nitrogen sources, phosphorus source, sylvite, filler described in the step (2) are:Account for fertilizer gross mass The potassium nitrate of 4.56%-22.67%, accounts for fertilizer gross mass at the monoammonium phosphate for accounting for fertilizer gross mass 2.92%-4.5% The potassium sulfate of 25.41%-9.26% accounts for fertilizer gross mass 2.8%-3.0% calcium superphosphate.
Preferably, ammonium nitrate accounts for the 82%-98% of gross mass in the ammonium nitrate phosphorus, and phosphorus pentoxide content contains in ammonium nitrate phosphorus It measures as 2%-8%.
Advantageous effect:
Different from the outer surface coating and cladding agent in granulated fertilizer, the present invention is promoted by limiting dispensing type with quantity The storage stability of nitro-compound fertilizer reduces the mass fraction of ammonium nitrate phosphorus (ANP) in dispensing, introduces potassium nitrate (KNO3) as fertilizer Second source of nitrate nitrogen in material, and the mass fraction of potassium sulfate is reduced in dispensing, while other dispensings are according to most preliminary design The nutrient content of fixed NPK is adjusted, and ensures that nitrogen, phosphorus, potassium nutrition content and nitrate nitrogen in formula be former and ammonium nitrogen In the case that ratio is basically unchanged, weaken nitro-compound fertilizer in cholesteric-nematic transition, improve fertilizer long-time storage stability and Caking performance avoids insoluble matter and resulting in blockage to drip irrigation facilities for oil product caused by excessively introducing coating agent and causes Economic loss.
Below by specific implementation, the present invention will be further described, but is not meant to the limit to the scope of the present invention System.
It is involved such as the methods of heating and drying in example below, it is that this field is normal if do not illustrated The method of rule;Equipment used and material are the equipment that this field can be obtained by commercial channel if do not illustrated And material.
Specific embodiment
Raw material:The raw material of fertilizer is the convenient source obtained by commercial channel in following comparative examples and embodiment;Nitre Sour potassium is the convenient source obtained by commercial channel;Ammonium nitrate accounts for the 82%-98% of gross mass in ammonium nitrate phosphorus, and phosphorus pentoxide contains Amount content in ammonium nitrate phosphorus is 2%-8%.
Comparative example 1
Existing technique prepares 18-9-18SOP compound fertilizers, and its step are as follows:
(1) preparation of solid material
It accounts for the monoammonium phosphate (nutrient content 11-49) of fertilizer gross mass 2.14%, 33.78% potassium sulfate, 2.8% cross phosphorus Sour calcium, 40.39% ammonium nitrate phosphorus (nutrient content 32-4), after being stirred, by Belt Conveying to rotary drum granulator, obtaining Solid material;
(2) preparation of granule materials
By 3% liquid nitrogen (accounting for fertilizer gross mass, provided by liquefied ammonia), 6.88% phosphorus pentoxide (accounts for the total matter of fertilizer Amount, is provided by phosphoric acid), sulfate radical 4.97% (is provided) by sulfuric acid, after being sufficiently mixed in tubular reactor, obtains liquid phase object Material, be ejected into the solid material of step (1), in tubular reactor simultaneously be passed through cleaning solution for adjust granulation humidity, liquid Phase materials are coated with granulating particle with solid-phase material in rotary drum granulator;Liquid phase feed passes through the Flux Valve Control unit interval Addition;Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and steam is passed through to adjust Humidity is granulated, obtains granule materials;
(3) preparation of granular 18-9-18SOP compound fertilizers
Grain size is prepared as 2-4.8mm by drying, screening, cooling, package process in granule materials obtained by step (2) Granular complex fertilizer, grade be nitro 18-9-18.
Embodiment 1
A kind of preparation method of the 18-9-18SOP compound fertilizers with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 31.27%, 9.56% potassium nitrate, by wherein 5% nitric acid are accounted for Potassium and 31.27% ammonium nitrate phosphorus form common solution of the water content for 15 weight % or so, and 120 DEG C of constant temperature stir half an hour, will expect It dries, cool down and be crushed to 40 mesh hereinafter, forming powdered modified nitrate nitrogen;
(2) preparation of solid material
By in step (1) powdered modified nitrate nitrogen, account for fertilizer gross mass 4.56% potassium nitrate, account for fertilizer gross mass 2.92% monoammonium phosphate, the potassium sulfate for accounting for fertilizer gross mass 25.41% account for 2.8% calcium superphosphate of fertilizer gross mass, and stirring is mixed It closes, by Belt Conveying to rotary drum granulator, obtaining solid material;
(3) preparation of granule materials
The liquid nitrogen for accounting for fertilizer gross mass 4.5% (is accounted for fertilizer gross mass, provided by liquefied ammonia, similarly hereinafter), accounts for the total matter of fertilizer The phosphorus pentoxide (account for fertilizer gross mass, provided by phosphoric acid, similarly hereinafter) of amount 6.84% accounts for the sulfuric acid of fertilizer gross mass 10.22% Root (is provided, similarly hereinafter) by sulfuric acid, after being sufficiently mixed in tubular reactor, obtains liquid phase material, is ejected into the solid of step (2) In material, be passed through simultaneously in tubular reactor cleaning solution for adjust the humidity that is granulated, liquid phase material and solid-phase material turn Granulating particle is coated in drum comminutor;The addition that liquid phase feed passes through the Flux Valve Control unit interval;Steam passes through valve Door is adjusted manually, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is granulated humidity for adjusting, and obtains particulate matter Material;
(4) preparation of the 18-9-18SOP compound fertilizers with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the 18-9- of 2-4.8mm is obtained 18SOP granular complex fertilizers 1, grade are nitro 18-9-18.
Embodiment 2
A kind of preparation method of the 18-9-18SOP compound fertilizers with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus for accounting for fertilizer gross mass 22.16% is 19.12% potassium nitrate, by wherein 6.5% The ammonium nitrate phosphorus of potassium nitrate and 22.16 weight % form common solution of the water content for 15 weight % or so, and 90 DEG C of constant temperature stirrings half are small When, material is dried, is cooled down and is crushed to 40 mesh hereinafter, forming powdered modified nitrate nitrogen;
(2) preparation of solid material
By in step (1) powdered modified nitrate nitrogen, account for fertilizer gross mass 12.62% potassium nitrate, account for fertilizer gross mass 3.7% monoammonium phosphate, the potassium sulfate for accounting for fertilizer gross mass 17.06% account for 2.8% calcium superphosphate of fertilizer gross mass, account for fertilizer 7.53% ammonium sulfate of gross mass, is stirred, by Belt Conveying to rotary drum granulator, obtaining solid material;
(3) preparation of granule materials
By the liquid nitrogen for accounting for fertilizer gross mass 4.43%, account for the phosphorus pentoxide of fertilizer gross mass 6.82% and to account for fertilizer total The sulfate radical (being provided by sulfuric acid) of quality 9.96%, after being sufficiently mixed in tubular reactor, obtains liquid phase material, is ejected into step Suddenly in the solid material of (2), in tubular reactor simultaneously be passed through cleaning solution for adjust be granulated humidity, liquid phase material with admittedly Phase materials are coated with granulating particle in rotary drum granulator;The addition that liquid phase feed passes through the Flux Valve Control unit interval; Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is granulated humidity for adjusting, Obtain granule materials;
(4) preparation of the 18-9-18SOP compound fertilizers with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the particle for obtaining 2-4.8mm is answered Hefei material 2, grade are nitro 18-9-18.
Embodiment 3
A kind of preparation method of the 18-9-18SOP compound fertilizers with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 13.1% is accounted for, accounts for the potassium nitrate of fertilizer gross mass 28.67%, it will Wherein 4% potassium nitrate and 13.1% ammonium nitrate phosphorus form common solution of the water content for 15 weight % or so, 135 DEG C of constant temperature stirrings Material is dried, cooled down and is crushed to 40 mesh hereinafter, forming powdered modified nitrate nitrogen by half an hour;
(2) preparation of solid material
By in step (1) powdered modified nitrate nitrogen, the potassium nitrate, 4.5% phosphoric acid one that account for fertilizer gross mass 24.67% Ammonium, 8.72% potassium sulfate, 2.8% calcium superphosphate, 15.2% ammonium sulfate, after being stirred, by Belt Conveying to rotary drum In comminutor, solid material is obtained;
(3) preparation of granule materials
The liquid nitrogen of fertilizer gross mass 4.3% will be accounted for, 6.78% phosphorus pentoxide, 9.6% sulfate radical is anti-in tubular type It answers after being sufficiently mixed in device, obtains liquid phase material, be ejected into the solid material of step (2), lead to simultaneously in tubular reactor Enter cleaning solution for adjust the humidity that is granulated, liquid phase material and solid-phase material are coated with granulating particle in rotary drum granulator;Liquid phase The addition that raw material passes through the Flux Valve Control unit interval;Steam is adjusted manually by valve, and steam jet is inserted into solid phase In the material bed of material, being passed through for steam is granulated humidity for adjusting, and obtains granule materials;
(4) preparation of the 18-9-18SOP compound fertilizers with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the particle for obtaining 2-4.8mm is answered Hefei material 3, grade are nitro 18-9-18.
Embodiment 4
A kind of preparation method of the 18-9-18SOP compound fertilizers with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 13.1% is accounted for, accounts for the potassium nitrate of fertilizer gross mass 28.67%, it will Wherein 1.2% potassium nitrate and 13.1% ammonium nitrate phosphorus, after high-temperature fusion forms slurry, whitewashing cooling forms granular change Property nitrate nitrogen, average grain diameter 2.0mm;
(2) preparation of solid material
By in step (1) granular modified nitrate nitrogen, the potassium nitrate, 4.5% phosphoric acid one that account for fertilizer gross mass 27.67% Ammonium, 8.72% potassium sulfate, 2.8% calcium superphosphate, 15.2% ammonium sulfate, after being stirred, by Belt Conveying to rotary drum In comminutor, solid material is obtained;
(3) preparation of granule materials
The liquid nitrogen of fertilizer gross mass 4.3% will be accounted for, 6.78% phosphorus pentoxide, 9.6% sulfate radical is anti-in tubular type It answers after being sufficiently mixed in device, obtains liquid phase material, be ejected into the solid material of step (2), lead to simultaneously in tubular reactor Enter cleaning solution for adjust the humidity that is granulated, liquid phase material and solid-phase material are coated with granulating particle in rotary drum granulator;Liquid phase The addition that raw material passes through the Flux Valve Control unit interval;Steam is adjusted manually by valve, and steam jet is inserted into solid phase In the material bed of material, being passed through for steam is granulated humidity for adjusting, and obtains granule materials;
(4) preparation of the 18-9-18SOP compound fertilizers with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the particle for obtaining 2-4.8mm is answered Hefei material 4, grade are nitro 18-9-18.
Embodiment 5
A kind of preparation method of the 18-9-18SOP compound fertilizers with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 13.1% is accounted for, accounts for the potassium nitrate of fertilizer gross mass 28.67%, it will Wherein 4% potassium nitrate and 13.1% ammonium nitrate phosphorus form common solution, and 135 DEG C of constant temperature stir half an hour, are formed stable molten altogether Slurry;
(2) preparation of solid material
The potassium nitrate of fertilizer gross mass 24.67%, 4.5% monoammonium phosphate, 8.72% potassium sulfate, 2.8% mistake will be accounted for Calcium phosphate, 15.2% ammonium sulfate, after being stirred, by Belt Conveying to rotary drum granulator, obtaining original solid material;It will Mutual solution slip in step (1) is ejected by nozzle in original solid material, obtains solid material;
(3) preparation of granule materials
The liquid nitrogen of fertilizer gross mass 4.3% will be accounted for, 6.78% phosphorus pentoxide, 9.6% sulfate radical is anti-in tubular type It answers after being sufficiently mixed in device, obtains liquid phase material, be ejected into the solid material that step (2) obtains, it is same in tubular reactor When be passed through cleaning solution for adjust the humidity that is granulated, liquid phase material and solid-phase material are coated with granulating particle in rotary drum granulator; The addition that liquid phase feed passes through the Flux Valve Control unit interval;Steam is adjusted manually by valve, and steam jet is inserted into In the material bed of solid-phase material, being passed through for steam is granulated humidity for adjusting, and obtains granule materials;
(4) preparation of the 18-9-18SOP compound fertilizers with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the particle for obtaining 2-4.8mm is answered Hefei material 5, grade are nitro 18-9-18
Briquetting method:Uniformly screening 2.0-4.0mm nitro-compound fertilizer particles, are put into internal diameter 4cm, the cylinder barrel of high 5cm In, imposing a condition is:Ballast weight 10kg, -25 DEG C of cyclically-varyings of briquetting temperature 60 C, a length of 5 days during briquetting, in the setting Under the conditions of, loose granular ammonium nitrate can the hardened diameter 4cm into cylindricality bulk, the shearing force of blocky ammonium nitrate is bigger, says Isotropic disk knot is more serious, and the smaller hardened degree of explanation of shearing force is lighter, and briquetting is repeated 10 times, and 10 times shearing force is averaged.
Embodiment data analysis
The cross shear average value of granular complex fertilizer in embodiment 1,2,3,4,5 be respectively 55.86N, 29.88N, 25.42N, 21.69N, 22.68N;The cross shear average value of granular complex fertilizer in comparative example 1 is 100.66N.
Shearing force is bigger illustrate particle between cohesive force it is stronger, blocking compound fertilizer granules are more.Above-mentioned conclusion explanation, leads to The storage stability of nitro-compound fertilizer can be promoted by crossing restriction dispensing type and quantity, and technology of the invention is to improve composite fertilizer to prevent One effective innovative technology in caking field.
The present inventor is using instruments such as X-ray diffraction, differential scanning calorimeter, thermodilatometric analysis instrument, infrared spectrums to nitre The physical property of ammonium phosphorus (ANP) has carried out comprehensive analysis, finds ammonium nitrate phosphorus (ANP) in the storage stability and formula of nitro high nitrogen fertilizer Dosage and physical property have relationship, therefore carried out it is a series of experiment optimization is adjusted to nitro high-nitrogen compound fertilizer formula, it is right Ammonium nitrate phosphorus (ANP) is modified, and achieves good improvement, and the storage stability of nitro-compound fertilizer has obtained significantly It improves.
Different from the outer surface coating and cladding agent in granulated fertilizer, the side disclosed by the invention for improving fertilizer storage stability Method is started with from change fertilizer internal structure, under the premise of fertilizer nutrient content and nitrate nitrogen are with ammonium nitrogen constant rate, is led to Optimizing raw material type is crossed, the modification of early period is carried out to raw material, the type of optimization dispensing improves fertilizer storage with proportioning to reach The purpose of stability.Present invention introduces potassium nitrate to substitute the nitrate nitrogen in the original formulation of part in ammonium nitrate phosphorus, while using nitric acid Potassium is modified the ammonium nitrate phosphorus in formula, and application obscure portions potassium nitrate carries out molten pretreatment (modified ammonium nitrate phosphorus) altogether with ammonium nitrate phosphorus, It is granulated again with unclassified stores later, weakens the cholesteric-nematic transition in granulated fertilizer, promote fertilizer storage stability and anti-caking Ability.
The present invention promotes the storage stability of nitro-compound fertilizer by limiting dispensing type with quantity, and nitre is reduced in dispensing The mass fraction of ammonium phosphorus (ANP) introduces potassium nitrate (KNO3) second source as nitrate nitrogen in fertilizer, and reduced in dispensing The mass fraction of potassium sulfate, while other dispensings are adjusted according to the nutrient content of the NPK initially set up, ensure formula In nitrogen, phosphorus, potassium nutrition content and nitrate nitrogen original and ammonium nitrogen ratio be basically unchanged in the case of, weaken nitro-compound fertilizer in Cholesteric-nematic transition, improve the long-time storage stability and caking performance of fertilizer.

Claims (10)

1. a kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 10%-34%, the potassium nitrate of 9%-30%, by which part nitric acid are accounted for Potassium forms common solution with ammonium nitrate phosphorus, the constant temperature at 90-135 DEG C, and material is dried, cooled down and crushed by stirring, forms modified nitre state Nitrogen;
(2) preparation of solid material
By in the modification nitrate nitrogen obtained in step (1), remaining potassium nitrate and fertilizer formula other ammonium nitrogen sources, phosphorus source, Sylvite, filler are stirred, and mixed material is transported in rotary drum granulator by feed belt, obtains solid material;
(3) preparation of granule materials
The liquid nitrogen of fertilizer gross mass 4.3%-4.5% will be accounted for, accounts for the phosphorus pentoxide of fertilizer gross mass 6.78%-6.84%, The sulfate radical of fertilizer gross mass 9.6%-10.22% is accounted for, after being sufficiently mixed in tubular reactor, obtains liquid phase material, is sprayed Into the solid material of step (2), in tubular reactor simultaneously be passed through cleaning solution for adjust granulation humidity, liquid phase material Granulating particle is coated in rotary drum granulator with solid-phase material;The addition that liquid phase feed passes through the Flux Valve Control unit interval Amount;Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is wet for adjusting granulation Degree, obtains granule materials;
(4) preparation of the granular nitro high-nitrogen compound fertilizer with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the grain with high storage stability is obtained Shape nitro high-nitrogen compound fertilizer.
2. the preparation method of the granular nitro high-nitrogen compound fertilizer according to claim 1 with high storage stability, special Sign is:Part potassium nitrate described in the step (1) accounts for 2 weight %-35 weight % of ammonium nitrate phosphorus.
3. the preparation method of the granular nitro high-nitrogen compound fertilizer according to claim 1 with high storage stability, special Sign is:In the step (1), the modified nitrate nitrogen is powdery, and powder granularity is below 40 mesh.
4. the preparation method of the granular nitro high-nitrogen compound fertilizer according to claim 1 with high storage stability, special Sign is:In the step (1), mass percent of the ammonium nitrate phosphorus in fertilizer formula be 13.1%-31.27%, nitric acid The mass percent of potassium is 9.56%-28.67%.
5. a kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability, its step are as follows:
(1) melt process of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 10%-34%, the potassium nitrate of 9%-30%, by which part nitric acid are accounted for Potassium is with ammonium nitrate phosphorus by high-temperature fusion, and after forming slurry, whitewashing curing, cooling forms modified nitrate nitrogen;
(2) preparation of solid material
By in the modification nitrate nitrogen obtained in step (1), remaining potassium nitrate and fertilizer formula other ammonium nitrogen sources, phosphorus source, Sylvite, filler are stirred, and mixed material is transported in rotary drum granulator by feed belt, obtains solid material;
(3) preparation of granule materials
The liquid nitrogen of fertilizer gross mass 4.3%-4.5% will be accounted for, accounts for the phosphorus pentoxide of fertilizer gross mass 6.78%-6.84%, The sulfate radical of fertilizer gross mass 9.6%-10.22% is accounted for, after being sufficiently mixed in tubular reactor, obtains liquid phase material, is sprayed Into the solid material of step (2), in tubular reactor simultaneously be passed through cleaning solution for adjust granulation humidity, liquid phase material Granulating particle is coated in rotary drum granulator with solid-phase material;The addition that liquid phase feed passes through the Flux Valve Control unit interval Amount;Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is wet for adjusting granulation Degree, obtains granule materials;
(4) preparation of the granular nitro high-nitrogen compound fertilizer with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the grain with high storage stability is obtained Shape nitro high-nitrogen compound fertilizer.
6. the preparation method of the granular nitro high-nitrogen compound fertilizer according to claim 5 with high storage stability, special Sign is:Part potassium nitrate described in the step (1) accounts for 1 weight %-10 weight % of ammonium nitrate phosphorus.
7. the preparation method of the granular nitro high-nitrogen compound fertilizer according to claim 5 with high storage stability, special Sign is:Modified nitrate nitrogen is granular described in the step (1), and granularity is in below 2.8mm.
8. a kind of preparation method of the granular nitro high-nitrogen compound fertilizer with high storage stability, its step are as follows:
(1) the molten processing altogether of potassium nitrate and ammonium nitrate phosphorus
In fertilizer formula, the ammonium nitrate phosphorus of fertilizer gross mass 10%-34% is accounted for, the potassium nitrate of 9%-30% is permanent at 90-135 DEG C Temperature, stirring, forms stable common solution;
(2) preparation of solid material
By in the remaining potassium nitrate in step (1) and fertilizer formula other ammonium nitrogen sources, phosphorus source, sylvite, filler stirring it is mixed It closes, mixed material is transported to by feed belt in rotary drum granulator, obtains original solid material;By what is obtained in step (1) Solution is ejected by nozzle on original solid material altogether, is participated in bonding granulating, is obtained solid material;
(3) preparation of granule materials
The liquid nitrogen of fertilizer gross mass 4.3%-4.5% will be accounted for, accounts for the phosphorus pentoxide of fertilizer gross mass 6.78%-6.84%, The sulfate radical of fertilizer gross mass 9.6%-10.22% is accounted for, after being sufficiently mixed in tubular reactor, obtains liquid phase material, is sprayed Into the solid material of step (2), in tubular reactor simultaneously be passed through cleaning solution for adjust granulation humidity, liquid phase material Granulating particle is coated in rotary drum granulator with solid-phase material;The addition that liquid phase feed passes through the Flux Valve Control unit interval Amount;Steam is adjusted manually by valve, and steam jet is inserted into the material bed of solid-phase material, and being passed through for steam is wet for adjusting granulation Degree, obtains granule materials;
(4) preparation of the granular nitro high-nitrogen compound fertilizer with high storage stability
By granule materials obtained by step (3) by drying, screening, cooling, package process, the grain with high storage stability is obtained Shape nitro high-nitrogen compound fertilizer.
9. the preparation method of the granular nitro high-nitrogen compound fertilizer according to claim 8 with high storage stability, special Sign is:The part potassium nitrate accounts for 2 weight %-35 weight % of ammonium nitrate phosphorus.
10. the system of the granular nitro high-nitrogen compound fertilizer with high storage stability according to any one of claim 1-9 Preparation Method, it is characterised in that:
The granular nitro high-nitrogen compound fertilizer refers to N P and K total nutrient more than 40%, wherein nitrogen content ≤17%, and nitre State nitrogen accounts for more than 28% total nitrogen, and nitro-compound fertilizer particle size is in 2.0-4.8mm;
The grade of the granular nitro high-nitrogen compound fertilizer includes 22-8-10,20-10-10,17-17-17 or 18-9- 18;
Other ammonium nitrogen sources in the step (2), phosphorus source, sylvite, filler include liquefied ammonia, phosphoric acid, sulfuric acid, potassium sulfate, potassium chloride, Ammonium sulfate, monoammonium phosphate, calcium superphosphate and sepiolite;
Alternatively, other ammonium nitrogen sources, phosphorus source, sylvite, filler are in the step (2):Account for fertilizer gross mass 4.56%- 22.67% potassium nitrate, the monoammonium phosphate for accounting for fertilizer gross mass 2.92%-4.5% account for fertilizer gross mass 25.41%-9.26% Potassium sulfate, account for fertilizer gross mass 2.8%-3.0% calcium superphosphate;
Ammonium nitrate accounts for the 82%-98% of gross mass in the ammonium nitrate phosphorus, and phosphorus pentoxide content content in ammonium nitrate phosphorus is 2%- 8%.
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CN109265228A (en) * 2018-12-07 2019-01-25 中国-阿拉伯化肥有限公司 A kind of long-acting compound fertilizer and preparation method thereof
CN109384251A (en) * 2018-12-12 2019-02-26 青海盐湖工业股份有限公司 A kind of prilling process of potassium nitrate and its potassium nitrate granules of preparation
CN109400376A (en) * 2018-12-07 2019-03-01 中国-阿拉伯化肥有限公司 A kind of compound fertilizer and preparation method thereof suitable for supporting shrimp rice field
CN113501509A (en) * 2021-08-19 2021-10-15 云南云天化红磷化工有限公司 System and method for preparing 66% powdery monoammonium phosphate by one-step method

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CN104961535A (en) * 2015-06-19 2015-10-07 陕西博农农资有限公司 Potassium nitrate water-soluble compound fertilizer and method for manufacturing same
CN107141064A (en) * 2017-05-12 2017-09-08 中国-阿拉伯化肥有限公司 A kind of method for improving phosphorus-potassium nitrate fertilizer material agglomeration preventing performance

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CN101367682A (en) * 2008-09-28 2009-02-18 中国-阿拉伯化肥有限公司 Method for preparing complex fertilizer with mutual solution slip tubular reactor
CN103664301A (en) * 2013-12-23 2014-03-26 史丹利化肥股份有限公司 Tower-type melt granulation water-soluble fertilizer containing fulvic acid potassium macroelement and preparation method for fertilizer
CN104961535A (en) * 2015-06-19 2015-10-07 陕西博农农资有限公司 Potassium nitrate water-soluble compound fertilizer and method for manufacturing same
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CN109265228A (en) * 2018-12-07 2019-01-25 中国-阿拉伯化肥有限公司 A kind of long-acting compound fertilizer and preparation method thereof
CN109400376A (en) * 2018-12-07 2019-03-01 中国-阿拉伯化肥有限公司 A kind of compound fertilizer and preparation method thereof suitable for supporting shrimp rice field
CN109384251A (en) * 2018-12-12 2019-02-26 青海盐湖工业股份有限公司 A kind of prilling process of potassium nitrate and its potassium nitrate granules of preparation
CN113501509A (en) * 2021-08-19 2021-10-15 云南云天化红磷化工有限公司 System and method for preparing 66% powdery monoammonium phosphate by one-step method

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