CN104108968B - A kind of granulation process of nitrophosphate fertilizer - Google Patents
A kind of granulation process of nitrophosphate fertilizer Download PDFInfo
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Abstract
The present invention relates to a kind of granulation process of nitrophosphate fertilizer, belong to nitrophosphate fertilizer field, mainly comprise the steps：Lower heating by nitrophosphate fertilizer concentrate, the finished particle of nitrophosphate fertilizer or nitrophosphate fertilizer returning charge particle at 125~190 DEG C, sprays slurry by the rotary nozzle of high tower granulator, obtains nitrophosphate fertilizer particle.Compound fertilizer product obtained by this method, uniform particle sizes, product is smooth, mellow and full, have needle-like thawing hole, intensity height, nutrient to adjust as needed, with the higher market competitiveness.
Description
Technical field
The present invention relates to chemical industry fertilizer technology field, more particularly to a kind of granulation process of nitrophosphate fertilizer.
Background technology
In current China's chemical industry fertilizer technology field, no high tower nitrophosphate fertilizer manufacturing process.Early stage nitrophosphate fertilizer
Granulation mode is based on biaxial granulation, and company built up first set nitrophosphate fertilizer high tower and made later stage Norway Ao Da 80 year 20th century
Grain mode.Shanxi Tian Ji coal chemical industries group is still based on biaxial granulation machine technique, Henan Jin Kai share control takeovers group and Shandong gold
Honest ecological engineering Co., Ltd produces nitrophosphate fertilizer using mixed acid process, and the Granulation Equipments used is spray drum fluid bed work
Skill is granulated, and the country is without high tower nitrophosphate fertilizer prilling.
The content of the invention
The of the invention main nitrophosphate fertilizer poor appearance for putting forth effort to solve traditional nitrophosphate fertilizer twin shaft and slurry-spraying pelletizing technique productions,
The problem of product moisture is high.The present invention is combined with high-tower granulation technology and nitrophosphate fertilizer traditional processing technology, by NP
Melted with concentrate or common process nitrophosphate fertilizer product and nitrophosphate fertilizer returning charge, evaporation section moisture in melting process, then
Granulated again by comminutor, products obtained therefrom moisture is low, intensity is high, light circularity is good, product has aperture, soluble.
The present invention uses prilling process to starch high-tower granulation technique for complete feed, therefore the space of fertilizer nutrient allotment is big, and nitrogen can
It is 10%~30% to control nutrient scope, and the controllable nutrient scope of phosphorus is 5%~45%.
The object of the invention is achieved through the following technical solutions：
A kind of granulation process of nitrophosphate fertilizer, by nitrophosphate fertilizer concentrate, the finished particle of nitrophosphate fertilizer or nitric acid phosphorus
Lower heating of the fertile returning charge particle at 125~190 DEG C, sprays slurry by the rotary nozzle of high tower granulator, obtains nitrophosphate fertilizer
Particle.
Under conditions of any fluxing agent, 125 DEG C of nitrophosphate fertilizer slurries begin to change into molten state, and more than 190 DEG C are adopted
With high-tower granulation technique of the present invention, ghost occurs in particle, is special-shaped grain, therefore temperature will be controlled at 125~190 DEG C.
It is preferred that, the preparation method of the nitrophosphate fertilizer concentrate comprises the following steps：The first step, nitric acid and phosphorus ore reaction system
Obtain acid hydrolysis solution；Second step, filtering；3rd step, the chilled crystallization of clear liquid after filtering separates out crystalline solid；4th step, except decrystallizing
Body；5th step, leads to ammonia with removing the clear liquid of crystal and carries out neutralization reaction；Slurry carries out multistage concentration system after 6th step, neutralization
Obtain in the nitrophosphate fertilizer that mass percent is 85%~98% and concentrate.
It is preferred that, the finished particle of the nitrophosphate fertilizer is the nitrophosphate fertilizer production that nitrophosphate fertilizer concentrate is obtained after granulation
Product.The preferred biaxial granulation machine of granulation mode, rotary drum granulator, granulating disc or oil bath comminutor.
It is preferred that, the nitrophosphate fertilizer returning charge particle is obtained returning charge of the nitrophosphate fertilizer concentrate after granulation, screening
Grain.The preferred biaxial granulation machine of granulation mode, rotary drum granulator, granulating disc or oil bath comminutor.
It is preferred that, also include screening and the processing of surface anti-caking after the rotary nozzle sprinkling slurry.
It is preferred that, the nitrophosphate fertilizer concentrate is delivered to tower top slurry storage tank by liquid conducting pipes.
It is preferred that, the finished particle and nitrophosphate fertilizer returning charge particle of the nitrophosphate fertilizer are that boosted machine is delivered to tower top slurry
Storage tank.
It is preferred that, the heating heats preferred steam-coil-heater using steam heating or electrical heating, steam.
It is preferred that, MAP, Diammonium phosphate (DAP) or sulphur ammonium are added according to the demand of crops, in the melting charge slurry to allocate
Nitrogen and phosphorus nutrients ratio, prepare nitrophosphate fertilizer master batch.
The present invention has the advantage that and beneficial effect relative to prior art：
(1) melting charge slurry moisture is low, without drying process, due to eliminating drying process and part cooling device,
Saved energy consumption, the equipment that the present invention is used have it is simple in construction, be easily installed and safeguard, the advantage of low cost；
(2) particle surface is smooth, mellow and full, prevented from caking, with the higher market competitiveness；
(3) good operational environment, three-waste free discharge belongs to process for cleanly preparing；
Brief description of the drawings
Fig. 1 is the technological process of production of nitrophosphate fertilizer concentrate high-tower granulation in embodiment 1；
Fig. 2 is the technological process of production of the embodiment 2 using the finished particle high-tower granulation of nitrophosphate fertilizer；
Fig. 3 is the technological process of production of the nitrophosphate fertilizer returning charge particle high-tower granulation of embodiment 3；
Fig. 4 is the nitrophosphate fertilizer particle that the embodiment of the present invention 1 is produced；
Fig. 5 is the nitrophosphate fertilizer particle of rotary drum fluid-bed technique productions；
Fig. 6 is the nitrophosphate fertilizer particle of day ridge biaxial granulation technique productions.
Above-mentioned Fig. 1：1- flotation ground phosphate rock；2-50% nitric acid；3- acid hydrolysis solutions；4- volutes machine, washing drum, filter press；5-
Insoluble matter；Clear liquid after 6- filterings；7- crystallizers；8-CN filters；9- four water-calcium nitrates；Clear liquid after 10- filterings；11- ammonias；
Slurry after 12- is neutralized；13- evaporators；14- nitrophosphate fertilizer concentrates；15- tower top slurry storage tanks；16- rotary nozzles；17- solids
Nitrophosphate fertilizer particle；18- vibratory sieves；19- packing machines 1#；20- packing machines；21- finished products；
Above-mentioned Fig. 2：1- flotation ground phosphate rock；2-50% nitric acid；3- acid hydrolysis solutions；4- volutes machine, washing drum, filter press；5-
Insoluble matter；Clear liquid after 6- filterings；7- crystallizers；8-CN filters；9- four water-calcium nitrates；Clear liquid after 10- filterings；11- ammonias；
Slurry after 12- is neutralized；13- evaporators；14- nitrophosphate fertilizer concentrates；22- biaxial granulation machines；23- bucket elevators；15- tower tops
Slurry storage tank；16- rotary nozzles；17- solid nitric acid phosphate fertilizer particles；18- vibratory sieves；19- packing machines 1#；20- packing machines 1#；
21- finished products；
Above-mentioned Fig. 3：1- flotation ground phosphate rock；2-50% nitric acid；3- acid hydrolysis solutions；4- volutes machine, washing drum, filter press；5-
Insoluble matter；Clear liquid after 6- filterings；7- crystallizers；8-CN filters；9- four water-calcium nitrates；Clear liquid after 10- filterings；11- ammonias；
Slurry after 12- is neutralized；13- evaporators；14- nitrophosphate fertilizer concentrates；22- biaxial granulation machines；24- vibratory sieves 2#；25- packing machines
2#；26- packing machines 2#；Good water solubility nitrophosphate fertilizer product low-grade 27-；The big returning charge particles of 28- and small returning charge particle；23-
Bucket elevator；15- tower top slurry storage tanks；16- rotary nozzles；17- solid nitric acid phosphate fertilizer particles；18- vibratory sieves；19- is wrapped up
Machine 1#；20- packing machines 1#；21- finished products.
Specific embodiment
The following example is further explanation of the present invention, and the present invention is not limited in any way.
Embodiment 1
As shown in figure 1, the first step, with the industrial nitric acid solution 2 and flotation phosphorus ore 1 that mass percent is 50% by weight
2.2:1 reaction, is made acid hydrolysis solution 3；Second step, acid hydrolysis solution is insoluble after being reacted by volute machine, washing drum and plate and frame filter press 4
Thing 5 is filtered；3rd step, the chilled crystallization of clear liquid 6 after filtering separates out the crystalline solid of four water-calcium nitrate 9；4th step, through CN filters
8 depth remove the four water-calcium nitrate 9 crystallized out；5th step, logical ammonia 11 carries out neutralizing instead with clear liquid 10 after filtration of calcium nitrate
Should；It is 92% nitrophosphate fertilizer concentration that slurry 12 carries out concentration mass percent is made by evaporator 13 after 6th step, neutralization
Liquid 14；7th step, nitrophosphate fertilizer concentrate 14 squeezes into 85m tower top slurries storage tank 15 for two grades through high pressure pumping point, through steam again
Coil pipe is heated to 170 DEG C of slurry solutions and concentrated again by whole level evaporator 13, and the nitric acid of mass percent 98% is made
Phosphate fertilizer slurry solution；8th step, slurry solution is flow to the rotary nozzle 16 of 80m comminutor by tremie pipe, in comminutor main shaft
Rotating speed is under the conditions of 100rpm, slurry liquid throws away from rotary nozzle 16, and slurry liquid is cold through the air that effective depth is 75m or so
But, the solid particle 17 that the crystallization of slurry liquid is diameter about 0.5~4.8mm；9th step, passes through the vibration that aperture is 2.0~4.0mm
Screen cloth sifts out 2.0~4.0mm finished particle, and the tenth step, finished particle is handled through anti-compaction, obtained product surface is mellow and full,
Particle is uniform, and product strength is high, the nitrophosphate fertilizer product 21 of good water solubility.
Using the granule strength of conventional rotary drum fluid-bed technique and biaxial granulation technique productions in below 35N, dissolving speed
Degree 6~8 minutes, Shanxi opens that board nitrophosphate fertilizer dissolution velocity is slower, nitrophosphate fertilizer particle appearance such as Fig. 5 and figure of common process production
Shown in 6；Dissolved 4.5 minutes using under the newton of nitrophosphate fertilizer finished particle intensity 50, quiescent conditions made from the inventive method, system
Product surface is more mellow and fuller, particle evenly, product appearance is as shown in Figure 4.
Embodiment 2
As shown in Fig. 2 the first step, with the industrial nitric acid solution 2 and flotation phosphorus ore 1 that mass percent is 50% by weight
Than 2.2:1 reaction, obtained acid hydrolysis solution 3, second step, acid hydrolysis solution is through passing through volute machine, washing drum and plate and frame filter press 4 after reacting
Insoluble matter 5 is filtered；3rd step, the chilled crystallization of clear liquid 6 after filtering separates out the crystalline solid of four water-calcium nitrate 9；4th step, through CN mistakes
The depth of filter 8 removes the four water-calcium nitrate 9 crystallized out；Clear liquid 10 after 5th step, logical ammonia 11 and filtration of calcium nitrate is carried out
Neutralization reaction；Slurry 12 carries out concentration by evaporator 13 and the nitric acid phosphorus that mass percent is 92% is made after 6th step, neutralization
0.5~5.2mm solid particle 17 is made through biaxial granulation machine 22 for fertile concentrate 14, the 7th step, nitrophosphate fertilizer concentrate 14, the
Eight steps, solid particle is carried to tower top through 125 DEG C of steam pipe coils progress heating meltings through bucket elevator 23, and the 9th step, slurry is molten
Liquid is flow to the rotary nozzle 16 of 80m comminutor by tremie pipe, the comminutor speed of mainshaft be 100rpm under the conditions of, slurry liquid from
Rotary nozzle 16 is thrown away, and slurry liquid is cooled down through the air that effective depth is 75m or so, the crystallization of slurry liquid for diameter about 0.5~
4.8mm solid particle 17, the tenth step, the sieved through sieve of vibratory sieve 18 through 2.0~4.0mm sifts out 2.0~4.0mm finished product
Grain, the 11st step, finished particle handles that obtained product surface is mellow and full, particle is uniform through anti-compaction, and product strength is high, water-soluble
Good nitrophosphate fertilizer product 21.
Dissolved 4.5 minutes under the newton of nitrophosphate fertilizer finished particle intensity 50, quiescent conditions, obtained product surface is more round
Profit, particle are evenly；Using the granule strength of conventional rotary drum fluid-bed technique productions in below 35N, 6~8 points of dissolution velocity
Clock, it is slower that nitrophosphate fertilizer dissolution velocity is opened in Shanxi.
Embodiment 3
As shown in figure 3, the first step, with the industrial nitric acid 2 and flotation phosphorus ore 1 that mass percent is 50% by weight 2.2:
1 reaction, obtained acid hydrolysis solution 3, second step, acid hydrolysis solution 3 is through passing through volute machine, washing drum and plate and frame filter press 4 insoluble after reacting
Thing 5 is filtered；3rd step, the chilled crystallization of clear liquid 6 after filtering separates out the crystalline solid of four water-calcium nitrate 9；4th step, through CN filters
8 depth remove the four water-calcium nitrate 9 crystallized out；5th step, leads to clear liquid 10 after ammonia 11 and filtering and carries out neutralization reaction；6th
Step, slurry 12 carries out concentration by evaporator 13 and the nitrophosphate fertilizer concentrate 14 that mass percent is 92% is made after neutralization；The
0.5~5.2mm solid particle is made through biaxial granulation machine 22 for seven steps, nitrophosphate fertilizer concentrate 14；8th step, solid particle warp
2.0~4.0mm vibratory sieve 2# mesh screens point, 2.0~4.0mm particles are dried through 125 DEG C of drying systems, after cooling, parcel, are entered
Row packaging, is made low-grade good water solubility nitrophosphate fertilizer product 27；9th step, through vibratory sieve 2#24 screen out 0.5~
4.1~5.2MM of 1.9MM small returning charge particle and vibratory sieve 2#24 extension sets screening big returning charge particle, big returning charge particle and small
Returning charge particle 28 carries to tower top through bucket elevator 23 and carries out heating meltings through 190 DEG C of steam pipe coils, the tenth step, slurry solution by
Tremie pipe flow to the rotary nozzle 16 of 80m comminutor, and under the conditions of the comminutor speed of mainshaft is 100rpm, slurry liquid is from rotation
Shower nozzle 16 is thrown away, and slurry liquid is cooled down through the air that effective depth is 75m or so, and the crystallization of slurry liquid is diameter about 0.5~4.8mm's
After solid particle, the 11st step, the sieved through sieve of vibratory sieve 18 through 2.0~4.0mm, obtained product surface is mellow and full, particle is equal
Even, product strength is high, the high-grade nitrophosphate fertilizer product 21 of good water solubility.
Dissolved 4.5 minutes under the newton of nitrophosphate fertilizer finished particle intensity 50, quiescent conditions, obtained product surface is more round
Profit, particle are evenly；Using conventional rotary drum fluid-bed technique dissolution velocity 6~8 minutes or so；Granule strength in below 35N,
It is slower that nitrophosphate fertilizer dissolution velocity is opened in Shanxi.
Claims (6)
1. a kind of granulation process of nitrophosphate fertilizer, it is characterised in that heat nitrophosphate fertilizer concentrate at 125~190 DEG C, leads to
The rotary nozzle sprinkling slurry of high tower granulator is crossed, nitrophosphate fertilizer particle is obtained,
Wherein, the preparation method of the nitrophosphate fertilizer concentrate comprises the following steps：
(1) with the industrial nitric acid solution and flotation phosphorus ore that mass percent is 50% by weight 2.2:1 reaction, is made acidolysis
Liquid；(2) insoluble matter is filtered after acid hydrolysis solution will be reacted by volute machine, washing drum and plate and frame filter press；(3) the clear liquid warp after filtering
Freezing and crystallizing separates out four water-calcium nitrate crystalline solid；(4) four water-calcium nitrate crystallized out is removed through CN filters depth；(5) lead to
Ammonia carries out neutralization reaction with clear liquid after filtration of calcium nitrate；(6) slurry carries out concentration by evaporator and quality hundred is made after neutralizing
Fraction is 92% nitrophosphate fertilizer concentrate；
The granulation process of the high tower granulator comprises the following steps：
Nitrophosphate fertilizer concentrate squeezes into 85m tower top slurry storage tanks through high pressure pumping, through steam-coil-heater again to 170 DEG C of slurries
Solution is concentrated again by whole level evaporator, and the nitrophosphate fertilizer slurry solution of mass percent 98% is made；Slurry solution
The rotary nozzle of 80m comminutor is flow to by tremie pipe, under the conditions of the comminutor speed of mainshaft is 100rpm, slurry liquid is from rotation
Shower nozzle is thrown away, and slurry liquid is cooled down through effective depth for 75m air, the solid that the crystallization of slurry liquid is 0.5~4.8mm of diameter
Grain；2.0~4.0mm finished particle is sifted out for 2.0~4.0mm vibration screen by aperture；Finished particle through anti-compaction at
Reason, obtained product surface is mellow and full, particle uniform, and product strength is high, the nitrophosphate fertilizer product of good water solubility.
2. granulation process according to claim 1, it is characterised in that：MAP, phosphoric acid are added in the slurry solution
Two ammoniums or sulphur ammonium allocate nitrogen and phosphorus nutrients ratio, prepare nitrophosphate fertilizer master batch.
3. a kind of granulation process of nitrophosphate fertilizer, it is characterised in that add the finished particle of nitrophosphate fertilizer at 125~190 DEG C
Heat, sprays slurry by the rotary nozzle of high tower granulator, obtains nitrophosphate fertilizer particle,
The preparation method of the finished particle of the nitrophosphate fertilizer comprises the following steps：
(1) with the industrial nitric acid solution and flotation phosphorus ore that mass percent is 50% by weight 2.2:1 reaction, is made acidolysis
Liquid, (2) acid hydrolysis solution is through filtering insoluble matter after reaction by volute machine, washing drum and plate and frame filter press；(3) clear liquid after filtering
Chilled crystallization separates out four water-calcium nitrate crystalline solid；(4) four water-calcium nitrate crystallized out is removed through CN filters depth；(5)
Clear liquid after logical ammonia and filtration of calcium nitrate carries out neutralization reaction；(6) slurry carries out concentration by evaporator and matter is made after neutralizing
Measure the nitrophosphate fertilizer concentrate that percentage is 92%；(7) nitrophosphate fertilizer concentrate obtains 0.5~5.2mm's through biaxial granulation mechanism
Solid particle；
The granulation process of the high tower granulator comprises the following steps：
By the finished particle of nitrophosphate fertilizer through bucket elevator carry to tower top through steam pipe coil carry out heating melting, slurry solution by
Tremie pipe flow to the rotary nozzle of 80m comminutor, and under the conditions of the comminutor speed of mainshaft is 100rpm, slurry liquid is from rotation spray
Head is thrown away, and slurry liquid is cooled down through effective depth for 75m air, the solid particle that the crystallization of slurry liquid is 0.5~4.8mm of diameter,
After vibrating screen mesh screening through 2.0~4.0mm, finished particle is handled through anti-compaction, and obtained product surface is mellow and full, particle is equal
Even, product strength is high, the high-grade nitrophosphate fertilizer product of good water solubility.
4. granulation process according to claim 3, it is characterised in that：MAP, phosphoric acid are added in the slurry solution
Two ammoniums or sulphur ammonium allocate nitrogen and phosphorus nutrients ratio, prepare nitrophosphate fertilizer master batch.
5. a kind of granulation process of nitrophosphate fertilizer, it is characterised in that heat nitrophosphate fertilizer returning charge particle at 125~190 DEG C,
Slurry is sprayed by the rotary nozzle of high tower granulator, nitrophosphate fertilizer particle is obtained,
The preparation method of the nitrophosphate fertilizer returning charge particle comprises the following steps：
(1) with the industrial nitric acid and flotation phosphorus ore that mass percent is 50% by weight 2.2:1 reaction, is made acid hydrolysis solution；(2)
Acid hydrolysis solution is through filtering insoluble matter after reaction by volute machine, washing drum and plate and frame filter press 4；(3) clear liquid after filtering is through cold
Freeze partial crystallization and go out four water-calcium nitrate crystalline solid；(4) four water-calcium nitrate crystallized out is removed through CN filters depth；(5) ammonia is led to
Clear liquid carries out neutralization reaction after gas and filtering；(6) slurry is by the obtained mass percent of evaporator progress concentration after neutralizing
92% nitrophosphate fertilizer concentrate；(7) nitrophosphate fertilizer concentrate obtains 0.5~5.2mm solid particle through biaxial granulation mechanism；
(8) vibratory sieve 2# mesh screen point of the solid particle through 2.0~4.0mm, 2.0~4.0mm particles are dried through 125 DEG C of drying systems, warp
After cooling, parcel, packed, low-grade good water solubility nitrophosphate fertilizer product is made；(9) screened out through vibratory sieve 2#
4.1~5.2mm of 0.5~1.9mm small returning charge particle and vibratory sieve 2# extension sets screening big returning charge particle；
The granulation process of the high tower granulator comprises the following steps：
By nitrophosphate fertilizer returning charge particle, carried through bucket elevator to tower top and carry out heating melting through steam pipe coil, slurry solution by
Tremie pipe flow to the rotary nozzle of 80m comminutor, and under the conditions of the comminutor speed of mainshaft is 100rpm, slurry liquid is from rotation spray
Head is thrown away, and slurry liquid is cooled down through effective depth for 75m air, the solid particle that the crystallization of slurry liquid is 0.5~4.8mm of diameter,
After vibrating screen mesh screening through 2.0~4.0mm, finished particle is handled through anti-compaction, and obtained product surface is mellow and full, particle is equal
Even, product strength is high, the high-grade nitrophosphate fertilizer product of good water solubility.
6. granulation process according to claim 5, it is characterised in that：MAP, phosphoric acid are added in the slurry solution
Two ammoniums or sulphur ammonium allocate nitrogen and phosphorus nutrients ratio, prepare nitrophosphate fertilizer master batch.
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| CN105777274A (en) * | 2015-03-31 | 2016-07-20 | 贵州芭田生态工程有限公司 | Preparation method of nanometer synergic urea nitro phosphate |
| CN105859369A (en) * | 2015-03-31 | 2016-08-17 | 贵州芭田生态工程有限公司 | Method for preparing nitro phosphate containing medium trace elements and polyphosphate |
| CN105859329A (en) * | 2015-03-31 | 2016-08-17 | 贵州芭田生态工程有限公司 | Method for preparing nitro phosphate containing polyphosphate and multiple nutrient elements |
| CN106380232A (en) * | 2016-08-19 | 2017-02-08 | 贵州芭田生态工程有限公司 | A nitrogen-phosphorous composite fertilizer and a preparing method thereof |
| CN110734314A (en) * | 2018-07-19 | 2020-01-31 | 贵州芭田生态工程有限公司 | Phosphorus potassium nitrate fertilizer and preparation method thereof |
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| CN101486595B (en) * | 2009-02-25 | 2011-03-30 | 天脊煤化工集团股份有限公司 | Technological process for producing high concentration nitric-phosphate fertilizer |
| CN102126738B (en) * | 2011-01-20 | 2012-11-28 | 山东金正大生态工程股份有限公司 | Method for producing nitrophosphate fertilizer and co-producing gypsum through decomposing phosphorite with nitric acid |
| CN102126741B (en) * | 2011-01-20 | 2012-11-28 | 山东金正大生态工程股份有限公司 | Method for producing nitro/S-based compound fertilizer and coproducing plaster |
| CN102351590B (en) * | 2011-07-18 | 2013-07-24 | 贵州省化工研究院 | Method for producing high-water solubility nitrophosphate fertilizer by phosphorite nitrolysis and calcium nitrate freezing |
| CN102992911A (en) * | 2012-12-31 | 2013-03-27 | 深圳市芭田生态工程股份有限公司 | Fertilizer and preparation method thereof |
| CN103073344B (en) * | 2013-01-23 | 2014-10-15 | 天脊煤化工集团股份有限公司 | Production method for high-concentration defluorinate nitronitrogen phosphorus and potassium compound fertilizer |
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