CN107381599A - A kind of bulky grain ammonium nitrate products and preparation method thereof - Google Patents
A kind of bulky grain ammonium nitrate products and preparation method thereof Download PDFInfo
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- CN107381599A CN107381599A CN201710814712.0A CN201710814712A CN107381599A CN 107381599 A CN107381599 A CN 107381599A CN 201710814712 A CN201710814712 A CN 201710814712A CN 107381599 A CN107381599 A CN 107381599A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/18—Nitrates of ammonium
- C01C1/185—Preparation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/21—Attrition-index or crushing strength of granulates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention provides a kind of bulky grain ammonium nitrate products and preparation method thereof and system; by using revolving drum granulator; make ammoniumnitrate prill move in circles the concentration liquid of ammonium nitrate after being atomized cladding; rear concentration liquid of ammonium nitrate is wrapped by every time and is able to crystallisation solidification on ammoniumnitrate prill surface, until ammoniumnitrate prill grows to the size of needs.For the bulky grain ammonium nitrate particle size of acquisition in more than 3mm, product storge quality is good, production process and system is safe and reliable, operating cost is low.
Description
Technical field
The invention belongs to the production technical field of ammonium nitrate, and in particular to a kind of bulky grain ammonium nitrate products and its system
Preparation Method and system.
Background technology
Ammonium nitrate products mainly use, product category mainly has multi-hole nitramines, liquid in civil explosive industry at present as commodity
Ammonium nitrate, industrial ammonium nitrate (high tower production little particle ammonium nitrate), crystallization ammonium nitrate.Wherein multi-hole nitramines are mainly for the manufacture of commerical grade and scene
Load in mixture a grade ammonium nitrate-fuel oil mixture, liquid ammonium nitrate, industrial ammonium nitrate, crystallize ammonium nitrate purposes it is roughly the same, available for manufacture emulsion, swollen
Change explosive, aqueous gels etc..
Liquid ammonium nitrate is that have the advantages of easy to use, its shortcoming is as commodity after directly ammonium nitrate solution is concentrated
It should not store for a long time.It is that vacuum crystallization is carried out after ammonium nitrate solution is concentrated to crystallize ammonium nitrate, obtains powdered crystalline product, the production
Product are very easy to moisture absorption caking, and it is big and dangerous to crush workload using preceding needing to be crushed by user.Industrial ammonium nitrate is handle
High tower is delivered to after ammonium nitrate solution concentration to be granulated, and obtains 1~2.8mm grain products, the grain products are smaller, Wu Fasheng
A length of bulky grain product, easy moisture absorption caking is stored for a long time.Multi-hole nitramines are usually using industrial ammonium nitrate or crystallize ammonium nitrate as raw material,
The techniques such as foamed, heat treatment are prepared, and surface has loose hole, is limited by its raw material granularity, granularity typically exists
Between 0.5~2.5mm, moisture absorption caking also easily occurs.
The content of the invention
In view of this, the invention is directed to a kind of bulky grain ammonium nitrate products and preparation method thereof, production process
It is safe and reliable with system, operating cost is low, product storge quality is good.
The granular ammonium nitrate of the invention, granularity is in more than 3mm, preferably 3~5mm.Further, the ammonium nitrate tool
There is mean compressive strength more than 20N/ particles；Free water content is in below 0.25wt%；Under conditions of not adding agglomeration agent, pine
Divergence is more than 95%.
The invention additionally provides a kind of preparation method of bulky grain ammonium nitrate, including following granulation steps：Make nitric acid
Ammonium particle moves in circles be atomized after concentration liquid of ammonium nitrate cladding, be wrapped by rear concentration liquid of ammonium nitrate every time in ammoniumnitrate prill
Surface is able to crystallisation solidification, until ammoniumnitrate prill grows to the size of needs.
Wherein, the temperature of the concentration liquid of ammonium nitrate is at 170 ± 5 DEG C, and concentration is wrapped by preceding nitre in more than 97wt% every time
Sour ammonium particle is through supercooling so that crystallization heat to be taken away.
Wherein, the ammoniumnitrate prill be wrapped by, crystallisation solidification and cooling process autonomous closure reaction compartment
Interior progress, it is in micro-vacuum state in control reaction compartment, preferable pressure is -50~-100Pa, and reaction compartment is worked off one's feeling vent one's spleen body temperature
Spend for 60-80 DEG C.
Wherein, ammoniumnitrate prill move in circles be wrapped by, crystallisation solidification and cooling process can be in revolving drum granulator
Middle completion, preferably using disclosed in notification number CN 203728738U, 23 days July in 2014 of the day for announcing, " a kind of rotating cylinder is granulated
Machine ".
Wherein, it is common crystallization ammonium nitrate, industry to move in circles by the ammoniumnitrate prill of concentration liquid of ammonium nitrate cladding
Ammonium nitrate derives from the nitric acid using this method growth using the granulation returning charge in this method preparation process, the granulation returning charge
The unqualified particle screened out in ammonium particle.
Wherein, the concentration liquid of ammonium nitrate is obtained using following step：
(1) neutralization procedure：Concentration 60wt% dust technology and gas ammonia are subjected to neutralization reaction under an increased pressure, obtained dense
Spend 75~80wt% ammonium nitrate solution, while by-product low-pressure steam, subsequent step is delivered to after the low-pressure steam of by-product is scrubbed
Use；
(2) first evaporation step：Using the low-pressure steam heating evaporation ammonium nitrate solution of neutralization procedure by-product, evaporator uses
Vacuum falling film is evaporated, and ammonium nitrate solution is concentrated into 92~95wt%；
(3) whole evaporation step：Normal pressure is used using from middle pressure steam heating evaporation ammonium nitrate solution out-of-bounds, evaporator
Evaporation, >=97wt% is concentrated to by ammonium nitrate solution.
Wherein, after the granulation step, in addition to screening step.The screening step be preferably divided into one-level screening step and
Two level screening step；One-level screening step is to screen out underproof little particle and bulky grain with double-deck screen shale shaker or rotary screen,
After bulky grain is broken and little particle is together as granulation returning charge；Two level screening step is to use individual layer or double-deck screen shale shaker or rotary screen
Finished particle is continued to screen out the bulky grain ammonium nitrate products of different grain size scope.
Wherein, after the screening step, in addition to finished product cooling step.Finished particle temperature is down to less than 45 DEG C.
Wherein, method of the invention also includes vent gas treatment step.By tail gas generated by granulation, screening tail gas and cooled exhaust gas washing
After processing, gas qualified discharge, cleaning solution is reclaimed.
Present invention also offers a kind of production system of bulky grain ammonium nitrate products, including the rotating cylinder being sequentially connected is granulated
Machine, particle conveyer, particle lifting machine and rotary screen, the rotary screen be provided with bulky grain discharging opening, finished particle discharging opening and
Little particle discharging opening, the bulky grain discharging opening is through disintegrating machine and little particle the discharging opening together returning charge entrance with revolving drum granulator
Connection, finished particle discharging opening are connected with finished particle elevator and storehouse cooler in turn.
Wherein, circulation is provided with outside the storehouse cooler, recirculated water enters the cooler that puts in storage from storehouse cooler bottom and followed
Ring, and sent out from the top of the cooler of storehouse.
Wherein, the production system is provided with vapo(u)rization system, including the first evaporator being serially connected and whole evaporator, the end
The discharging opening of evaporator connects with the atomizer of revolving drum granulator.
Wherein, the production system is additionally provided with scrubbing tower, and the tail gas of the revolving drum granulator, rotary screen and storehouse cooler passes through
Pipeline is connected with the scrubbing tower, and the gas up to standard of scrubbing tower is back to by tower top discharge, the condensed water of scrubbing tower by pipeline
First evaporator and/or whole evaporator.
Relative to prior art, the invention has the advantage that：Bulky grain nitre of the granularity in more than 3mm can be provided
Sour ammonium product, product anti-caking performance is good, and storage stability is high, and compression strength is high and shatter value is high.Production method and production are
System is safe and reliable, and operating cost is low.
Brief description of the drawings
The accompanying drawing for forming the part of the invention is used for providing further understanding the invention, present invention wound
The schematic description and description made is used to explain the invention, does not form the improper restriction to the invention.
In accompanying drawing：
Fig. 1 is the structural representation of the invention production system.
Embodiment
The invention is described more detail below.
The granular ammonium nitrate of the invention, granularity is in more than 3mm, preferably 3~5mm.Further, the ammonium nitrate tool
There is mean compressive strength more than 20N/ particles；Free water content is in below 0.25wt%；Under conditions of not adding agglomeration agent, pine
Divergence is more than 95%.Bulky grain ammonium nitrate products index provided by the invention and the contrast of existing product index are as shown in table 1.
Table 1
The preparation method of the above-mentioned bulky grain ammonium nitrate of the invention, including following granulation steps：Follow ammoniumnitrate prill
Concentration liquid of ammonium nitrate after ring is back and forth atomized coats, and is wrapped by rear concentration liquid of ammonium nitrate every time and is able on ammoniumnitrate prill surface
Crystallisation solidification, until ammoniumnitrate prill grows to the size of needs.
Wherein, in order that the concentration liquid of ammonium nitrate obtained after coating every time quickly can smoothly crystallize on ammoniumnitrate prill surface
, it is necessary to control the temperature of concentration liquid of ammonium nitrate at 170 ± 5 DEG C, concentration is wrapped by preceding ammonium nitrate in more than 97wt% every time for solidification
For particle through supercooling so that crystallization heat to be taken away, preferable cooling medium is normal temperature air.
Wherein, for the purpose of safety anti-explosive, ammoniumnitrate prill is wrapped by, crystallisation solidification and cooling process needs
Carried out in the reaction compartment of autonomous closure, be in micro-vacuum state in control reaction compartment, preferable pressure for -50~-
100Pa, reaction compartment exit gas (tail gas) temperature are 60-80 DEG C.Micro-vacuum state is advantageous to prevent pressure in reaction compartment
Safety problem caused by excessive, while be advantageous to the rapid crystallization of particle and grow up；The adjustment of pressure can realize by circulating air,
The air inlet of circulating air is can be used as generally as the normal temperature air of cooling medium, while is used as and follows from space a part of tail gas of extraction
The outlet of ring gas, tail gas can be as an index of temperature on average in reflection reaction compartment, on the whole control reaction compartments
Interior state of temperature, controlled in suitable temperature, may advantageously facilitate the progress of granular grows.Tail gas can by recycling
To collect ammonium nitrate therein, put back into and (will be described further below in vent gas treatment step) as raw material.
Wherein, ammoniumnitrate prill move in circles be wrapped by, crystallisation solidification and cooling process can be in revolving drum granulator
Middle completion, preferably using disclosed in notification number CN 203728738U, 23 days July in 2014 of the day for announcing, " a kind of rotating cylinder is granulated
Machine ".Atomizer is provided with the revolving drum granulator, rises and lifts the parts such as flight, fluid bed, cooler, returning charge spiral.Rotating cylinder is made
When grain machine rotates, rise act flight and ammoniumnitrate prill is constantly sent into fluid bed, the fluidisation bedside that ammoniumnitrate prill is obliquely installed certainly
Along falling, material curtain is formed.Ammoniumnitrate prill in rolling process, sprays on fluid bed with the cooler set in self-fluidized type bed
Cooling air carries out heat exchange cooling.Concentration liquid of ammonium nitrate is uniformly coated on what is fallen in material curtain formula after nozzle height is atomized
On ammoniumnitrate prill and solidify.Ammoniumnitrate prill constantly repeats above-mentioned during being granulated in machine drum body to port of export movement
Granulation process, particle are gradually grown up.Space in revolving drum granulator is the reaction compartment of ammoniumnitrate prill, passes through circulation in space
Gas maintains -50~-100Pa micro-vacuum state, and the cooling air that cooler sprays is circulating air air inlet, and outlet tail gas is circulation
The outlet of gas.
Wherein, move in circles by concentration liquid of ammonium nitrate cladding the ammoniumnitrate prill can be common crystallization ammonium nitrate,
Industrial ammonium nitrate is preferably to use the granulation returning charge in this method preparation process, and the granulation returning charge, which derives from, uses this method
(unqualified little particle can be unqualified big directly as granulation returning charge for the unqualified particle screened out in the ammoniumnitrate prill of growth
Particle can be used as be granulated returning charge after crushing).The screening of unqualified particle can be carried by reaction compartment (or revolving drum granulator)
Returning charge or grading plant carry out, the screening plant that is separately provided after can also being discharged by autoreaction space (or revolving drum granulator)
Carry out.For example, above-mentioned revolving drum granulator is internally provided with returning charge spiral and classfied cone, classfied cone is located at the port of export, to particle certainly
Dynamic classification, little particle deliver to comminutor entrance point through returning charge spiral, can so ensure that the returning charge amount outside revolving drum granulator is protected
A very low level is held, outside screening, broken, revert system investment can be reduced (such as the screening being separately provided after discharging
Equipment), and mitigate the abrasion of equipment.
Wherein, the concentration liquid of ammonium nitrate is obtained using following step：
(1) neutralization procedure：Concentration 60wt% dust technology and gas ammonia are subjected to neutralization reaction under an increased pressure, obtained dense
Spend 75~80wt% ammonium nitrate solution, while by-product low-pressure steam, subsequent step is delivered to after the low-pressure steam of by-product is scrubbed
Use；
(2) first evaporation step：Using the low-pressure steam heating evaporation ammonium nitrate solution of neutralization procedure by-product, evaporator uses
Vacuum falling film is evaporated, and ammonium nitrate solution is concentrated into 92~95wt%；
(3) whole evaporation step：Normal pressure is used using from middle pressure steam heating evaporation ammonium nitrate solution out-of-bounds, evaporator
Evaporation, >=97wt% is concentrated to by ammonium nitrate solution.
The acquisition process of above-mentioned concentration liquid of ammonium nitrate, the heat of reaction system can be made full use of, be evaporated by two steps,
The concentration liquid of ammonium nitrate of aimed concn is obtained under lowest energy consumption.
Wherein, after the granulation step, in addition to screening step.The screening step be preferably divided into one-level screening step and
Two level screening step.One-level screening step is to screen out underproof little particle and bulky grain with double-deck screen shale shaker or rotary screen,
After bulky grain is broken and little particle is together as granulation returning charge；The qualified finished particle of granularity delivers to subsequent process steps.Two level
Screening step is that finished particle is continued to sieve with individual layer or double-deck screen shale shaker or rotary screen, several different grain size scopes of output
Bulky grain ammonium nitrate products；Particle size range is illustrated：3~3.5mm scopes, 3.5~5mm scopes；Or, 3~4mm scopes, 4~5mm
Scope；Particle size range can determine as needed.When need not segment finished product grain graininess scope, two level screening step can be disabled
Suddenly, the finished particle of one-level screening step is fed directly to subsequent process steps.
Wherein, after the screening step, in addition to finished product cooling step.After screening, the temperature of finished particle about 100~
110℃.Finished particle cooling step uses bin type cooler, vertical, and inside is provided with 3 groups of plate type heat exchangers, finished product
Grain passes sequentially through 3 groups of plate type heat exchangers from top to bottom, and recirculated cooling water passes sequentially through 3 groups of plate type heat exchangers, finished product from bottom to top
Particle and recirculated cooling water indirect heat exchange, are down to less than 45 DEG C, in favor of packing and storing by finished particle temperature.
Wherein, method of the invention also includes vent gas treatment step.Tail gas generated by granulation, screening tail gas and cooled exhaust gas dust contain
Measure higher, about 15~20g/m3, scrubbing tower carrying out washing treatment can be used.Because dust is ammonium nitrate in tail gas, it is water-soluble
Very well, dust content≤30mg/m can be made after scrubbing tower is washed with water3, qualified discharge.Scrubbing tower is equipped with cleaning circulation pump and followed
Washing-round is washed.Supplement water of the process condensate water of first/whole evaporation step of ammonium nitrate as scrubbing tower, after cleaning solution concentration reaches 30wt%
First/whole evaporation step of ammonium nitrate is delivered to be reclaimed.
Present invention also offers a kind of production system of bulky grain ammonium nitrate products, such as Fig. 1, including the rotating cylinder being sequentially connected
Comminutor 1, particle conveyer 2, particle lifting machine 3 and rotary screen 4, the rotary screen 4 are provided with bulky grain discharging opening 41, finished product
Grain discharging opening 42 and little particle discharging opening 43, the bulky grain discharging opening 41 through disintegrating machine 5 and little particle discharging opening 43 together with
The returning charge entrance 11 of revolving drum granulator 1 connects, and finished particle discharging opening 42 is connected with finished particle elevator 6 and storehouse cooler in turn
7.Particle is transported to rotary screen 4 and sieved through particle conveyer 2, particle lifting machine 3 successively after the granulation of revolving drum granulator 1,
The unqualified bulky grain screened out is sent out from bulky grain discharging opening 41, after disintegrating machine 5 is broken, with being sieved from little particle discharging opening 43
The unqualified little particle separated is granulated again together as returning charge into revolving drum granulator 1, the qualified finished product screened out
Grain is sent out from finished particle discharging opening 42, is cooled down through the cooler 7 that enters to put in storage of finished particle elevator 6, turns into production eventually after cooling
Product can be packaged output.
Wherein, the outside of the storehouse cooler 7 is provided with circulation, and recirculated water is carried out from the bottom of storehouse cooler 7 cooler 7 that enters to put in storage
Circulation, and sent out from the top of storehouse cooler 7.
Wherein, the production system is provided with vapo(u)rization system, including the first evaporator 8 and whole evaporator 9 being serially connected, described
The discharging opening of whole evaporator 9 connects with the atomizer 12 of revolving drum granulator 1.Ammonium nitrate solution after neutralization is admitted to just evaporation
Device 8, and just evaporation step and whole evaporation step are carried out in first evaporator 8 and whole evaporator 9 respectively, reach the concentration of needs
(>=97wt%), it is then fed into revolving drum granulator 1 and is atomized ejection through atomizer 12, carries out granulation step.
Wherein, the production system is additionally provided with scrubbing tower 10, the tail of the revolving drum granulator 1, rotary screen 4 and storehouse cooler 7
Gas is connected by pipeline with the scrubbing tower 10, and the gas up to standard of scrubbing tower 10 is led to by tower top discharge, the condensed water of scrubbing tower 10
Piping is back to just evaporator 8 and/or whole evaporator 9, may be repeated recycling.
The preferred embodiment of the invention is the foregoing is only, is not intended to limit the invention creation, it is all at this
Within the spirit and principle of innovation and creation, any modification, equivalent substitution and improvements made etc., the invention should be included in
Protection domain within.
Claims (10)
1. a kind of granular ammonium nitrate, granularity is in more than 3mm, preferably 3~5mm.
2. granular ammonium nitrate according to claim 1, it is characterised in that the ammonium nitrate has more than 20N/ particles flat
Equal compression strength；Free water content is in below 0.25wt%；Under conditions of not adding agglomeration agent, shatter value is more than 95%.
3. a kind of preparation method of bulky grain ammonium nitrate, including following granulation steps：Make ammoniumnitrate prill move in circles to be atomized
Concentration liquid of ammonium nitrate cladding afterwards, is wrapped by rear concentration liquid of ammonium nitrate and is able to crystallisation solidification on ammoniumnitrate prill surface, directly every time
The size of needs is grown to ammoniumnitrate prill.
4. the preparation method of bulky grain ammonium nitrate according to claim 3, it is characterised in that the concentration liquid of ammonium nitrate
Temperature at 170 ± 5 DEG C, concentration in more than 97wt%, before being wrapped by every time ammoniumnitrate prill through supercooling with by crystallization heat band
Walk.
5. the preparation method of bulky grain ammonium nitrate according to claim 3, it is characterised in that the ammoniumnitrate prill is wrapped
Cover, crystallisation solidification and cooling process carried out in the reaction compartment of autonomous closure, control reaction compartment in be in tiny structure shape
State, preferable pressure are -50~-100Pa, and reaction compartment Outlet Gas Temperature is 60-80 DEG C.
6. the preparation method of bulky grain ammonium nitrate according to claim 3, it is characterised in that move in circles dense by ammonium nitrate
The ammoniumnitrate prill of contracting liquid cladding is common crystallization ammonium nitrate, industrial ammonium nitrate or uses making in this method preparation process
Grain returning charge, the unqualified particle for being granulated returning charge and being screened out in the ammoniumnitrate prill using this method growth.
7. the preparation method of bulky grain ammonium nitrate according to claim 3, it is characterised in that the concentration liquid of ammonium nitrate is adopted
Obtained with following step：
(1) neutralization procedure：Concentration 60wt% dust technology and gas ammonia are subjected to neutralization reaction under an increased pressure, obtain concentration 75
~80wt% ammonium nitrate solution, while by-product low-pressure steam, subsequent step use is delivered to after the low-pressure steam of by-product is scrubbed；
(2) first evaporation step：Using the low-pressure steam heating evaporation ammonium nitrate solution of neutralization procedure by-product, evaporator uses vacuum
Falling film evaporation, ammonium nitrate solution is concentrated to 92~95wt%；
(3) whole evaporation step：Steamed using from middle pressure steam heating evaporation ammonium nitrate solution out-of-bounds, evaporator using normal pressure
Hair, >=97wt% is concentrated to by ammonium nitrate solution.
8. the preparation method of bulky grain ammonium nitrate according to claim 3, it is characterised in that after the granulation step, also
Including screening step.The screening step is preferably divided into one-level screening step and two level screening step；One-level screening step is to use
Double-deck screen shale shaker or rotary screen screen out underproof little particle and bulky grain, with little particle together as making after bulky grain is broken
Grain returning charge；Two level screening step is that finished particle is continued with individual layer or double-deck screen shale shaker or rotary screen to screen out different grain size model
The bulky grain ammonium nitrate products enclosed.
9. the preparation method of bulky grain ammonium nitrate according to claim 3, it is characterised in that after the screening step, also
Including finished product cooling step.Finished particle temperature is down to less than 45 DEG C.
10. the preparation method of bulky grain ammonium nitrate according to claim 3, it is characterised in that method of the invention is also wrapped
Include vent gas treatment step.After tail gas generated by granulation, screening tail gas and cooled exhaust gas carrying out washing treatment, gas qualified discharge, cleaning solution enters
Row recovery.
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Cited By (3)
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| CN109020771A (en) * | 2018-08-29 | 2018-12-18 | 佛山朝鸿新材料科技有限公司 | A kind of preparation method of heat-resisting anti-caking ammonium nitrate |
| CN112624153A (en) * | 2021-01-08 | 2021-04-09 | 四川金象赛瑞化工股份有限公司 | Porous ammonium nitrate production process |
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| CN109019645A (en) * | 2018-09-25 | 2018-12-18 | 天津华景化工新技术开发有限公司 | A kind of production system and production method of bulky grain magnesium nitrate |
| CN109019645B (en) * | 2018-09-25 | 2023-07-14 | 天津华景工程技术有限公司 | Production system and production method of large-particle magnesium nitrate |
| CN112624153A (en) * | 2021-01-08 | 2021-04-09 | 四川金象赛瑞化工股份有限公司 | Porous ammonium nitrate production process |
| CN112624153B (en) * | 2021-01-08 | 2022-10-14 | 四川金象赛瑞化工股份有限公司 | Porous ammonium nitrate production process |
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