CN110903108A - Production method for increasing 64% diammonium phosphate nitrogen content and ammoniation granulator - Google Patents
Production method for increasing 64% diammonium phosphate nitrogen content and ammoniation granulator Download PDFInfo
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- CN110903108A CN110903108A CN201911357270.7A CN201911357270A CN110903108A CN 110903108 A CN110903108 A CN 110903108A CN 201911357270 A CN201911357270 A CN 201911357270A CN 110903108 A CN110903108 A CN 110903108A
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- diammonium phosphate
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 42
- ZRIUUUJAJJNDSS-UHFFFAOYSA-N ammonium phosphates Chemical compound [NH4+].[NH4+].[NH4+].[O-]P([O-])([O-])=O ZRIUUUJAJJNDSS-UHFFFAOYSA-N 0.000 title description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 147
- 239000005696 Diammonium phosphate Substances 0.000 claims abstract description 112
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims abstract description 112
- 235000019838 diammonium phosphate Nutrition 0.000 claims abstract description 112
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 105
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 100
- 239000000463 material Substances 0.000 claims abstract description 85
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000005406 washing Methods 0.000 claims abstract description 67
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 62
- 238000001035 drying Methods 0.000 claims abstract description 45
- 239000007789 gas Substances 0.000 claims abstract description 44
- 238000005469 granulation Methods 0.000 claims abstract description 43
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 38
- 230000003179 granulation Effects 0.000 claims abstract description 36
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 35
- 239000002002 slurry Substances 0.000 claims abstract description 30
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 238000012216 screening Methods 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 15
- 239000011248 coating agent Substances 0.000 claims description 41
- 238000000576 coating method Methods 0.000 claims description 41
- 239000004254 Ammonium phosphate Substances 0.000 claims description 39
- 229910000148 ammonium phosphate Inorganic materials 0.000 claims description 39
- 235000019289 ammonium phosphates Nutrition 0.000 claims description 39
- 238000009423 ventilation Methods 0.000 claims description 14
- 238000004176 ammonification Methods 0.000 claims description 7
- 239000000428 dust Substances 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 18
- 238000005054 agglomeration Methods 0.000 abstract description 5
- 230000002776 aggregation Effects 0.000 abstract description 5
- 230000000903 blocking effect Effects 0.000 abstract description 5
- 239000012895 dilution Substances 0.000 abstract description 5
- 238000010790 dilution Methods 0.000 abstract description 5
- 239000003337 fertilizer Substances 0.000 description 32
- 239000012071 phase Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 14
- 241000406668 Loxodonta cyclotis Species 0.000 description 10
- 230000008569 process Effects 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 239000007792 gaseous phase Substances 0.000 description 6
- 229920002643 polyglutamic acid Polymers 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 108010020346 Polyglutamic Acid Proteins 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- -1 diammonium phosphate compound Chemical class 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 239000002689 soil Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 4
- 230000002195 synergetic effect Effects 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 3
- RQFQJYYMBWVMQG-IXDPLRRUSA-N chitotriose Chemical compound O[C@@H]1[C@@H](N)[C@H](O)O[C@H](CO)[C@H]1O[C@H]1[C@H](N)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)N)[C@@H](CO)O1 RQFQJYYMBWVMQG-IXDPLRRUSA-N 0.000 description 3
- 229940044175 cobalt sulfate Drugs 0.000 description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 235000015097 nutrients Nutrition 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 230000009466 transformation Effects 0.000 description 3
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- YRPFQANFEPFYSJ-UHFFFAOYSA-N [K].[B].[Zn] Chemical compound [K].[B].[Zn] YRPFQANFEPFYSJ-UHFFFAOYSA-N 0.000 description 2
- 229940038879 chelated zinc Drugs 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 244000068988 Glycine max Species 0.000 description 1
- 235000010469 Glycine max Nutrition 0.000 description 1
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 240000003768 Solanum lycopersicum Species 0.000 description 1
- 244000061456 Solanum tuberosum Species 0.000 description 1
- 235000002595 Solanum tuberosum Nutrition 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 244000098338 Triticum aestivum Species 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- CDMADVZSLOHIFP-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 CDMADVZSLOHIFP-UHFFFAOYSA-N 0.000 description 1
- RSCACTKJFSTWPV-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane;pentahydrate Chemical compound O.O.O.O.O.[Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 RSCACTKJFSTWPV-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229940095686 granule product Drugs 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 235000019837 monoammonium phosphate Nutrition 0.000 description 1
- 239000006012 monoammonium phosphate Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 235000021048 nutrient requirements Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000002786 root growth Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B19/00—Granulation or pelletisation of phosphatic fertilisers, other than slag
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/003—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic followed by coating of the granules
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a production method for increasing the nitrogen content of 64% diammonium phosphate, which comprises the following steps: and the pipe counter pump sends phosphoric acid in the pipe counter tank to the mixer to perform a first neutralization reaction with liquid ammonia, and then the phosphoric acid is uniformly sprayed in the ammoniation granulator, so that slurry and the liquid ammonia sent by the ammonia distributor perform a second neutralization reaction, and after granulation is completed in the ammoniation granulator, the diammonium phosphate particle product with higher nitrogen content is obtained through parallel-flow heat exchange drying, screening, cooling and wrapping. The method solves the problem of gas phase short circuit in the granulator, reduces the concentration of water vapor in the granulator, reduces the degree of pre-washing neutralization, stably controls the degree of pipe reverse neutralization, increases the degree of secondary ammoniation neutralization, and improves the content of N in 64 percent diammonium phosphate products; the N content of 64 percent diammonium phosphate products produced by the ammoniation granulator is more than 17.80 percent, the water content is reduced, the phenomena of pipe reverse blocking, granulator dilution running, material agglomeration and the like are effectively inhibited, and the start-up rate is improved.
Description
Technical Field
The invention belongs to the technical field of agricultural fertilizer manufacturing, and particularly relates to a production method for increasing the content of 64% diammonium phosphate nitrogen and an ammoniation granulator.
Background
The ammoniation granulation process has the characteristics of less investment, strong operability, high productivity, low energy consumption and low production cost, and is a production process widely applied to the field of compound fertilizer production. The process is roughly as follows: the raw materials are metered, crushed and uniformly mixed according to a corresponding proportion, then are sent into an ammoniation granulator and are sprayed on a rolling granulating material bed, an ammonia distributor is embedded in the granulating material bed, gas ammonia is sprayed into the granulating material bed through the ammonia distributor, and material particles on the ammonia distributor are neutralized again to achieve the purposes of particle sizing and nitrogen nutrient increase.
The production of diammonium phosphate (DAP) can be achieved by neutralization reaction of dilute phosphoric acid and ammonia, or by ammoniation of concentrated phosphoric acid under the condition of pressurization and temperature rise. When ammonia and phosphoric acid are aminated in the tubular reactor, the heat of neutralization reaction can raise the slurry temperature to above 150 deg.C, and its steam pressure is up to 0.2Kgf/cm2Above, byUnder the self-pressure, the ammonium phosphate slurry can be directly sprayed into a granulation spray tower to produce granular powdery ammonium phosphate.
In the production process of diammonium phosphate (DAP), the neutralization degree has a certain relation with the pH value, but the method is not similar to pure H3PO4Relative relationship in reaction with ammonia to pure H3PO4In general, H is3PO4The neutralization degree of the first hydrogen ion in the ammonium phosphate solution is 1, the molar ratio is 1, the pH of the 0.1 concentration is 4.4, and H is3PO4The neutralization degree of the second hydrogen ion is 2 when the second hydrogen ion is completely neutralized into diammonium phosphate by ammonia, the molar ratio is 2, the pH value of 0.2 concentration is 8.0, in actual production, due to the existence of other impurities in phosphoric acid and the impossibility of completely neutralizing the second hydrogen ion, the neutralization degree is generally less than 2, and the pH value is also less than 8.0, which is the reason that 100 percent diammonium phosphate (DAP) product cannot be obtained in production, but diammonium phosphate (DAP) product containing a small amount of MAP.
The degree of neutralization is the molar ratio of the amino acids, and the control of the degree of neutralization is accomplished by measurement. In the production process of diammonium phosphate (DAP), the pH value is an extremely important control index, and the pH value has great influence on the properties of slurry and the granulation operation. The optimum degree of neutralization should be as low as possible loss of ammonia during neutralization, so that the amount of liquid phase in the neutralized slurry is minimized and the slurry has good fluidity, thereby facilitating the subsequent granulation and washing processes.
The vapor pressure of ammonia increases significantly with the degree of neutralization, e.g., at 75 deg.C, at a neutralization level of 1.5, the vapor pressure of ammonia is 0.19 KPa; when the neutralization degree is 1.7, the ammonia partial pressure is 0.7 KPa; when the neutralization degree is 1.9, the ammonia partial pressure is 4.1 KPa; from the viewpoint of reducing ammonia loss, the neutralization degree is controlled to be lower, but the neutralization degree is too low, the liquid phase amount in slurry is increased, great difficulty is brought to drying and granulation, such as dilution, material blockage, energy consumption increase and the like, and even the required diammonium phosphate (DAP) product cannot be obtained.
When the temperature is 75 ℃, the solubility of MAP is maximum, the solubility is reduced along with the increase of the neutralization degree, the viscosity is increased, when the neutralization degree exceeds 1.0, diammonium phosphate (DAP) is formed to increase the solubility of the ammonium phosphate, and when the neutralization degree is 1.4-1.5, the solubility is maximum, and the slurry flowability is best.
As the granular diammonium is adopted by the tubular reactor, the neutralization process is completed in one step, the escaped ammonia accounts for about 30-35% of the total ammonia feeding amount, and the granular diammonium needs to be washed and recovered by concentrated acid, in the washing process, the phosphoric acid absorbs the ammonia to generate monoammonium phosphate, the neutralization degree in a concentrated acid tank is higher and higher along with the washing, in order to ensure that the washing acid and the production acid have good fluidity, the neutralization degree of the washing acid is controlled to be between 0.5 and 0.7, the pH value is smaller than 2, a pre-neutralization ammoniation granulation process is adopted for a newly-built diammonium device, and the pre-neutralization degree is controlled to be between 1.4 and 1.5, so that slurry with good fluidity can be obtained.
Currently, there are some methods disclosed for the production and processing of diammonium phosphate, for example:
1. patent application CN201910589537.9 discloses a diammonium phosphate compound fertilizer and a preparation method and application thereof, and active ingredients of the compound fertilizer comprise the following components: polyglutamic acid, chitosan oligosaccharide, titanium dioxide and diammonium phosphate; wherein the mass of the polyglutamic acid is 0.01-0.5 per mill of the mass of the diammonium phosphate; the mass of the chitosan oligosaccharide is 0.3-1 per mill of the mass of diammonium phosphate; the mass of the titanium dioxide is 0.1-0.5 per mill of the mass of the diammonium phosphate. The diammonium phosphate compound fertilizer can reasonably adjust the proportion of the gamma-polyglutamic acid, the chitosan oligosaccharide and the titanium dioxide according to the nutrient requirements of different crops, release organic nutrients in soil, improve the utilization rate of the fertilizer, enhance the stress resistance of the crops, promote the growth of the crops and improve the yield and the quality of the crops.
2. Patent application CN201910144697.2 discloses a diammonium phosphate compound fertilizer and a preparation method thereof, wherein active ingredients of the compound fertilizer comprise diammonium phosphate, polyglutamic acid and cobalt sulfate; wherein, the mass of the polyglutamic acid is 0.02 per thousand to 1 per thousand of the mass of the diammonium phosphate; the mass of the cobalt sulfate is 2-5% of that of the diammonium phosphate. The invention can control the release period of the compound fertilizer by adjusting the proportion of polyglutamic acid and cobalt sulfate, and can prolong the release time of the fertilizer, improve the utilization rate of the fertilizer and effectively improve the crop yield by developing a quick-acting fertilizer and a long-acting fertilizer; meanwhile, the microbial state of the soil can be improved, the microbial diversity of the soil can be increased, and the soil hardening caused by fertilizer application can be effectively improved. The diammonium phosphate compound fertilizer can be used as base fertilizer, top dressing fertilizer and hole fertilizer, and can be applied by root application and irrigation. It is suitable for grain crops such as wheat, corn and rice, and also suitable for economic crops such as tomato, potato, grape and soybean.
3. Patent application CN201810612619.6 discloses an energy-gathering chelated zinc boron-potassium-rich diammonium phosphate fertilizer and a preparation method thereof, wherein the energy-gathering chelated zinc boron-potassium-rich diammonium phosphate fertilizer comprises the following raw material components in parts by weight: 30-60 parts of compound amino acid, 15-25 parts of soluble zinc salt, 10-15 parts of carboxymethyl cellulose, 5-10 parts of urea, 2-5 parts of pectin, 10-30 parts of chelating agent, 40-55 parts of borax pentahydrate, 5-8 parts of borax decahydrate, 2-5 parts of concentrated sulfuric acid, 15-20 parts of potassium chloride, 0.1-0.3 part of trace element, 40-55 parts of concentrated phosphoric acid, 5-10 parts of ammonium sulfate, 1-2 parts of boric acid, 2-5 parts of ammonia water and 300 parts of water 170. Has the advantages that: the fertilizer processing flow is simplified, the processing time is shortened, the labor intensity of workers is reduced, the fertilizer efficiency is stable, lasting and slow, the utilization rate of the fertilizer is improved, and the use cost is reduced.
4. Patent application CN201610944094.7 discloses a diammonium phosphate synergistic fertilizer and a preparation method thereof. The synergistic fertilizer consists of diammonium phosphate and a diammonium phosphate synergist, wherein the content of diammonium phosphate in the synergistic fertilizer is 98-99%, and the content of the diammonium phosphate-containing synergist is 1-2%; the diammonium phosphate synergist contains 14-16% of humic acid, 0.01-0.02% of zinc and 0.02-0.03% of boron, the pH value is 9-11, and the phosphorus fixation rate is reduced by at least 20%. The diammonium phosphate synergistic fertilizer formed by the coordination of the diammonium phosphate and the synergist has the characteristics of obvious effect of reducing phosphorus fixation, greatly improving phosphorus activity, promoting crop root growth, improving root activity, remarkably increasing crop yield, improving fertilizer utilization rate, being environment-friendly, supplementing soil trace elements and the like. And the preparation process is simple, the raw material source is wide, the operation is easy, the cost is low, and the like.
However, the above patent applications and other publications aim to increase the content of active ingredients of fertilizers by adding other fertilizer ingredients besides phosphorus and nitrogen, and thus the nitrogen content of the fertilizers meets the domestic industrial standards but still cannot meet the international market requirements.
In addition, the ammoniation granulation process has the characteristics of less investment, strong operability, high productivity, low energy consumption and low production cost, and is a production process widely applied to the field of compound fertilizer production. The process is roughly as follows: the raw materials are metered, crushed and uniformly mixed according to a corresponding proportion, then are sent into an ammoniation granulator and are sprayed on a rolling granulating material bed, an ammonia distributor is embedded in the granulating material bed, gas ammonia is sprayed into the granulating material bed through the ammonia distributor, and material particles on the ammonia distributor are neutralized again to achieve the purposes of particle sizing and nitrogen nutrient increase. Therefore, the ammonification granulator is used as an instrument required in the production process of the diammonium phosphate. The conventional ammoniation granulator has the following disadvantages: (1) the concentration of water vapor in the ammoniation granulator is high, a large amount of air outside the baffle door is gushed into the cavity of the granulator in a negative pressure state, the gas phase in the cavity of the granulator is easy to generate a short circuit phenomenon, the water vapor in the granulator cannot be extracted in time, the moisture of materials is higher, and the secondary ammoniation is difficult; and (2) the degree of neutralization in prewashing is relatively high (the degree of neutralization is less than 0.65 in the traditional process), the degree of neutralization in tube reaction and secondary ammoniation is relatively low (the degree of neutralization in tube reaction is 1.50-1.60 in the traditional process), the degree of neutralization is not easy to regulate and control, the content of N in the product is limited to be increased (the content of N in the traditional method is less than 17.8 percent), phenomena such as tube reverse blocking, granulator running dilution, material agglomeration and the like are prone to occurring frequently, and the ammoniation granulator is frequently stopped.
At present, the products produced by the traditional diammonium phosphate production process are regulated according to the national standard, wherein the effective phosphorus (P) is contained in the products2O5) The mass fraction is more than or equal to 46 percent, and the nitrogen (N) content is more than or equal to 17 percent. However, the phosphoric acid used as a raw material obtained by wet-process phosphoric acid concentration is affected by solid content, double-accompanying oxides and the like, so that the nitrogen content in the produced diammonium phosphate product is less than 18 percent, and the diammonium phosphate product does not meet the standards of foreign markets. By using the traditional production process of the preneutralization tubular reactor, the N content of the product diammonium phosphate is influenced by impuritiesIt is difficult to achieve 18% or more.
Disclosure of Invention
The invention provides a production method for improving the content of 64% diammonium phosphate nitrogen and an ammoniation granulator, which aim to solve the technical problems.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a production method for increasing the nitrogen content of 64% diammonium phosphate comprises the following steps:
step one, a pipe reverse pump sends phosphoric acid in a pipe reverse tank to a mixer to perform a first neutralization reaction with liquid ammonia to obtain slurry;
uniformly spraying the slurry into an ammoniation granulator, and performing secondary neutralization reaction on the slurry and liquid ammonia fed by an ammonia distributor to obtain an ammonium phosphate material;
and step three, after the ammonium phosphate material is granulated in an ammoniation granulator, performing parallel flow heat exchange drying, screening, cooling and wrapping to obtain a diammonium phosphate particle product with high nitrogen content.
Further, in the first step, the content of P2O5 in the phosphoric acid is 39% -41%.
Further, in the first step and the second step, the neutralization degree of the first neutralization reaction between the phosphoric acid and the liquid ammonia is 1.500-1.530; the neutralization degree of the second neutralization reaction is 1.85-1.90, and the water content of the ammonium phosphate material is 3.2% -3.65%.
Further, in the third step, the parallel-flow heat exchange drying is to send the ammonium phosphate material to a dryer to perform parallel-flow heat exchange drying with hot air from a hot-blast stove at 500-550 ℃, a gas phase in the ammoniation granulator is washed sequentially by a drying washing tower and a tail gas washing tower in the drying process, the tail gas washing tower is composed of a prewashing tower and a granulation washing tower, the gas phase firstly passes through the prewashing tower and then enters the granulation washing tower, and the drying washing tower and the granulation washing tower can absorb ammonia gas and dust.
Further, in the third step, the water content of the diammonium phosphate is 1.8% -2.5%.
Further, in step three, the three ways in which the ammonium phosphate material is converted into the diammonium phosphate granule product in the ammoniation granulator are coating, binding and self-granulation, wherein the coating granulation has the best appearance quality.
Further, in step three, the screening is performed by four stages of screening.
And further, in the step three, the cooling is to send the screened qualified materials into the fluidized bed through a chute, and then the materials are driven by cooling air to float and cool.
Further, in the third step, the coating is to send the cooled material into a coating machine through a chute, then uniformly coat the material with coating oil, and send the material into a finished product belt through the chute, wherein the mass ratio of the diammonium phosphate to the coating oil is 500: 0.9-1.2 during the coating.
Further, the ammoniation granulator for improving the nitrogen content of a 64% diammonium phosphate product comprises a return port, a tubular reactor, a baffle, a barrel, a gas phase outlet, a baffle door, a baffle discharge port, a baffle door movable observation port and a particle feed port, wherein the baffle is provided with a baffle vent, the return port is provided with a return port vent, and the return port vent is directly connected with a return port; the axial flow fan is arranged close to the return port ventilation opening and is connected with the return port through the return port ventilation opening; only two movable observation ports are arranged on the stop gate; the baffle vent is close to the tubular reactor and is far away from the baffle discharge hole.
The invention creatively improves the production process of diammonium phosphate, solves the problem of gas phase short circuit in a granulator, reduces the concentration of water vapor in the granulator, reduces the degree of pre-washing neutralization (the degree of neutralization is less than 0.45), stably controls the degree of tube reverse neutralization (the degree of tube reverse neutralization is 1.500-1.530), increases the degree of secondary ammoniation neutralization (the degree of neutralization of secondary ammoniation is 1.85-1.90), and improves the content of N in 64 percent diammonium phosphate products.
Carry out technical transformation to the ammoniation granulator, close four movable shutter viewing apertures in ammoniation granulator shutter top, stop the gaseous phase short circuit, in addition, add the blow vent at ammoniation granulator baffle, add vent and axial fan at ammoniation granulator feed back mouth, reduce the interior steam enrichment of ammoniation granulator cavity, increase gaseous phase flow, ensure the interior little negative pressure state of ammoniation granulator simultaneously, stop the ammonia and escape, cause ammonia loss and safety ring to protect the risk.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
(1) the method has the advantages that the production process of diammonium phosphate is creatively improved, the problem of gas phase short circuit in a granulator is solved, the concentration of water vapor in the granulator is reduced, the pre-washing neutralization degree (the neutralization degree is less than 0.45) is reduced, the tube reverse neutralization degree (the tube reverse neutralization degree is 1.500-1.530) is stably controlled, the secondary ammoniation neutralization degree (the secondary ammoniation neutralization degree is 1.85-1.90) is increased, and the content of N in 64% diammonium phosphate products is increased.
(2) The N content of 64% diammonium phosphate products produced by the ammoniation granulator is more than 17.80%, the moisture content is reduced, the requirement of various complex component source acid indexes can be met, the phenomena of pipe reverse blocking, granulator dilution running, material agglomeration and the like are effectively restrained, and the start-up rate is improved.
(3) This application is to prior art's shortcoming, carry out technical transformation to the ammoniation granulator, close four movable shutter viewing apertures in ammoniation granulator shutter top, stop the gaseous phase short circuit, in addition, add the blow vent at ammoniation granulator baffle, add vent and axial fan at ammoniation granulator returning charge mouth, reduce the interior steam enrichment of ammoniation granulator cavity, increase the gaseous phase and flow, ensure the interior micro-negative pressure state of ammoniation granulator simultaneously, stop the ammonia and escape, cause ammonia loss and safety ring to protect the risk.
Drawings
In order to illustrate the embodiments of the present invention or the technical solutions in the prior art more clearly, the drawings needed in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some examples of the present invention, and for a person skilled in the art, without inventive step, other drawings can be obtained according to these drawings:
FIG. 1 is a schematic view of an ammoniation granulator according to the present application;
FIG. 2 is a schematic view of the configuration of the ammoniation granulator baffle of the present application;
FIG. 3 is a schematic structural view of a shutter of the ammoniation granulator of the present application;
FIG. 4 is a schematic structural diagram of an ammoniation granulator in comparative example 1;
FIG. 5 is a schematic structural diagram of a baffle of an ammoniation granulator of comparative example 1;
fig. 6 is a schematic structural diagram of a shutter of the ammonification granulator of comparative example 1.
In the drawings: 1-returning a material port; 2-a tubular reactor; 3-a baffle plate; 4-a cylinder body; 5-gas phase outlet; 6-a stop gate; 7-baffle discharge port; 8-movable observation port of the stop gate; 9-granule feed opening; 10-baffle vent; 11-a return port vent; 12-axial flow fan.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
A production method for increasing the nitrogen content of 64% diammonium phosphate comprises the following steps:
step one, a pipe reverse pump sends phosphoric acid in a pipe reverse tank to a mixer to perform a first neutralization reaction with liquid ammonia to obtain slurry; p in the phosphoric acid2O5The content is 39%;
uniformly spraying the slurry into an ammoniation granulator, and performing secondary neutralization reaction on the slurry and liquid ammonia fed by an ammonia distributor to obtain an ammonium phosphate material;
thirdly, after the ammonium phosphate material is granulated in an ammoniation granulator, performing parallel flow heat exchange drying, screening, cooling and wrapping to obtain a diammonium phosphate granular product with high nitrogen content;
the parallel-flow heat exchange drying is to send ammonium phosphate materials to a dryer to perform parallel-flow heat exchange drying with hot air at 500 ℃ from a hot-blast stove, gas phase in an ammoniation granulator is washed sequentially by a drying washing tower and a tail gas washing tower in the drying process, the tail gas washing tower consists of a pre-washing tower and a granulation washing tower, the gas phase firstly passes through the pre-washing tower and then enters the granulation washing tower, and the drying washing tower and the granulation washing tower can absorb ammonia gas and dust; the water content of the diammonium phosphate is 1.8%; in an ammoniation granulator, three ways for the ammonium phosphate material to become a diammonium phosphate granular product are coating, bonding and self-granulation, wherein the coating granulation has the best appearance quality; the screening is carried out by four stages; the cooling is to send the screened qualified materials into a fluidized bed through a chute, and then to drive the materials to float and cool by cooling air; and the coating is to send the cooled material into a coating machine through an elephant trunk, then uniformly coat the material with coating oil, and send the material into a finished product belt through the elephant trunk, wherein the mass ratio of the diammonium phosphate to the coating oil is 500: 0.9.
Further, in the first step and the second step, the neutralization degree of the first neutralization reaction between the phosphoric acid and the liquid ammonia is 1.500; the neutralization degree of the second neutralization reaction is 1.85, and the water content of the ammonium phosphate material is 3.2%.
As shown in fig. 1, 2 and 3, the ammoniation granulator for increasing the nitrogen content of a 64% diammonium phosphate product comprises a return port 1, a tubular reactor 2, a baffle 3, a cylinder 4, a gas phase outlet 5, a baffle door 6, a baffle discharge port 7, a baffle door movable observation port 8 and a particle feed port 9, wherein the baffle 3 is provided with a baffle vent 10, the return port 1 is provided with a return port vent 11, and the return port vent 11 is directly connected with the return port 1; the axial flow fan 12 is arranged close to the return port ventilation opening 11, and the axial flow fan 12 is connected with the return port 1 through the return port ventilation opening 11; only two movable observation ports 8 are arranged; the baffle vent 10 is close to the tubular reactor 2 and remote from the baffle discharge opening 7.
Example 2
A production method for increasing the nitrogen content of 64% diammonium phosphate comprises the following steps:
step one, a pipe reverse pump sends phosphoric acid in a pipe reverse tank to a mixer to perform a first neutralization reaction with liquid ammonia to obtain slurry; p in the phosphoric acid2O5The content is 41%;
uniformly spraying the slurry into an ammoniation granulator, and performing secondary neutralization reaction on the slurry and liquid ammonia fed by an ammonia distributor to obtain an ammonium phosphate material;
thirdly, after the ammonium phosphate material is granulated in an ammoniation granulator, performing parallel flow heat exchange drying, screening, cooling and wrapping to obtain a diammonium phosphate granular product with high nitrogen content;
the parallel-flow heat exchange drying is to send ammonium phosphate materials to a dryer to perform parallel-flow heat exchange drying with hot air from a hot-blast stove at 550 ℃, gas phase in an ammoniation granulator is washed sequentially by a drying washing tower and a tail gas washing tower in the drying process, the tail gas washing tower consists of a pre-washing tower and a granulation washing tower, the gas phase firstly passes through the pre-washing tower and then enters the granulation washing tower, and the drying washing tower and the granulation washing tower can absorb ammonia gas and dust; the water content of the diammonium phosphate is 2.5%; in an ammoniation granulator, three ways for the ammonium phosphate material to become a diammonium phosphate granular product are coating, bonding and self-granulation, wherein the coating granulation has the best appearance quality; the screening is carried out by four stages; the cooling is to send the screened qualified materials into a fluidized bed through a chute, and then to drive the materials to float and cool by cooling air; and the coating is to send the cooled material into a coating machine through an elephant trunk, then uniformly coat the material with coating oil, and send the material into a finished product belt through the elephant trunk, wherein the mass ratio of the diammonium phosphate to the coating oil is 500:1.2 during the coating.
Further, in the first step and the second step, the neutralization degree of the first neutralization reaction between the phosphoric acid and the liquid ammonia is 1.530; the neutralization degree of the second neutralization reaction is 1.90, and the water content of the ammonium phosphate material is 3.65%.
As shown in fig. 1, 2 and 3, the ammoniation granulator for increasing the nitrogen content of a 64% diammonium phosphate product comprises a return port 1, a tubular reactor 2, a baffle 3, a cylinder 4, a gas phase outlet 5, a baffle door 6, a baffle discharge port 7, a baffle door movable observation port 8 and a particle feed port 9, wherein the baffle 3 is provided with a baffle vent 10, the return port 1 is provided with a return port vent 11, and the return port vent 11 is directly connected with the return port 1; the axial flow fan 12 is arranged close to the return port ventilation opening 11, and the axial flow fan 12 is connected with the return port 1 through the return port ventilation opening 11; only two movable observation ports 8 are arranged; the baffle vent 10 is close to the tubular reactor 2 and remote from the baffle discharge opening 7.
Example 3
A production method for increasing the nitrogen content of 64% diammonium phosphate comprises the following steps:
step one, a pipe reverse pump sends phosphoric acid in a pipe reverse tank to a mixer to perform a first neutralization reaction with liquid ammonia to obtain slurry; p in the phosphoric acid2O5The content is 39%;
uniformly spraying the slurry into an ammoniation granulator, and performing secondary neutralization reaction on the slurry and liquid ammonia fed by an ammonia distributor to obtain an ammonium phosphate material;
thirdly, after the ammonium phosphate material is granulated in an ammoniation granulator, performing parallel flow heat exchange drying, screening, cooling and wrapping to obtain a diammonium phosphate granular product with high nitrogen content;
the parallel-flow heat exchange drying is to send ammonium phosphate materials to a dryer to perform parallel-flow heat exchange drying with hot air from a hot-blast stove at 510 ℃, gas phase in an ammoniation granulator is washed sequentially by a drying washing tower and a tail gas washing tower in the drying process, the tail gas washing tower consists of a pre-washing tower and a granulation washing tower, the gas phase firstly passes through the pre-washing tower and then enters the granulation washing tower, and the drying washing tower and the granulation washing tower can absorb ammonia gas and dust; the water content of the diammonium phosphate is 1.9%; in an ammoniation granulator, three ways for the ammonium phosphate material to become a diammonium phosphate granular product are coating, bonding and self-granulation, wherein the coating granulation has the best appearance quality; the screening is carried out by four stages; the cooling is to send the screened qualified materials into a fluidized bed through a chute, and then to drive the materials to float and cool by cooling air; and the coating is to send the cooled material into a coating machine through an elephant trunk, then uniformly coat the material with coating oil, and send the material into a finished product belt through the elephant trunk, wherein the mass ratio of the diammonium phosphate to the coating oil is 500: 0.95.
Further, in the first step and the second step, the neutralization degree of the first neutralization reaction between the phosphoric acid and the liquid ammonia is 1.510; the neutralization degree of the second neutralization reaction is 1.86, and the water content of the ammonium phosphate material is 3.3%.
As shown in fig. 1, 2 and 3, the ammoniation granulator for increasing the nitrogen content of a 64% diammonium phosphate product comprises a return port 1, a tubular reactor 2, a baffle 3, a cylinder 4, a gas phase outlet 5, a baffle door 6, a baffle discharge port 7, a baffle door movable observation port 8 and a particle feed port 9, wherein the baffle 3 is provided with a baffle vent 10, the return port 1 is provided with a return port vent 11, and the return port vent 11 is directly connected with the return port 1; the axial flow fan 12 is arranged close to the return port ventilation opening 11, and the axial flow fan 12 is connected with the return port 1 through the return port ventilation opening 11; only two movable observation ports 8 are arranged; the baffle vent 10 is close to the tubular reactor 2 and remote from the baffle discharge opening 7.
Example 4
A production method for increasing the nitrogen content of 64% diammonium phosphate comprises the following steps:
step one, a pipe reverse pump sends phosphoric acid in a pipe reverse tank to a mixer to perform a first neutralization reaction with liquid ammonia to obtain slurry; p in the phosphoric acid2O5The content is 41%;
uniformly spraying the slurry into an ammoniation granulator, and performing secondary neutralization reaction on the slurry and liquid ammonia fed by an ammonia distributor to obtain an ammonium phosphate material;
thirdly, after the ammonium phosphate material is granulated in an ammoniation granulator, performing parallel flow heat exchange drying, screening, cooling and wrapping to obtain a diammonium phosphate granular product with high nitrogen content;
the parallel-flow heat exchange drying is to send ammonium phosphate materials to a dryer to perform parallel-flow heat exchange drying with hot air from a hot-blast stove at 540 ℃, gas phase in an ammoniation granulator is washed sequentially by a drying washing tower and a tail gas washing tower in the drying process, the tail gas washing tower consists of a pre-washing tower and a granulation washing tower, the gas phase firstly passes through the pre-washing tower and then enters the granulation washing tower, and the drying washing tower and the granulation washing tower can absorb ammonia gas and dust; the water content of the diammonium phosphate is 2.3%; in an ammoniation granulator, three ways for the ammonium phosphate material to become a diammonium phosphate granular product are coating, bonding and self-granulation, wherein the coating granulation has the best appearance quality; the screening is carried out by four stages; the cooling is to send the screened qualified materials into a fluidized bed through a chute, and then to drive the materials to float and cool by cooling air; and the coating is to send the cooled material into a coating machine through an elephant trunk, then uniformly coat the material with coating oil, and send the material into a finished product belt through the elephant trunk, wherein the mass ratio of the diammonium phosphate to the coating oil is 500:1.1 during the coating.
Further, in the first step and the second step, the neutralization degree of the first neutralization reaction between the phosphoric acid and the liquid ammonia is 1.520; the neutralization degree of the second neutralization reaction is 1.89, and the water content of the ammonium phosphate material is 3.5%.
As shown in fig. 1, 2 and 3, the ammoniation granulator for increasing the nitrogen content of a 64% diammonium phosphate product comprises a return port 1, a tubular reactor 2, a baffle 3, a cylinder 4, a gas phase outlet 5, a baffle door 6, a baffle discharge port 7, a baffle door movable observation port 8 and a particle feed port 9, wherein the baffle 3 is provided with a baffle vent 10, the return port 1 is provided with a return port vent 11, and the return port vent 11 is directly connected with the return port 1; the axial flow fan 12 is arranged close to the return port ventilation opening 11, and the axial flow fan 12 is connected with the return port 1 through the return port ventilation opening 11; only two movable observation ports 8 are arranged; the baffle vent 10 is close to the tubular reactor 2 and remote from the baffle discharge opening 7.
Example 5
A production method for increasing the nitrogen content of 64% diammonium phosphate comprises the following steps:
step one, a pipe reverse pump sends phosphoric acid in a pipe reverse tank to a mixer to perform a first neutralization reaction with liquid ammonia to obtain slurry; p in the phosphoric acid2O5The content is 40 percent;
uniformly spraying the slurry into an ammoniation granulator, and performing secondary neutralization reaction on the slurry and liquid ammonia fed by an ammonia distributor to obtain an ammonium phosphate material;
thirdly, after the ammonium phosphate material is granulated in an ammoniation granulator, performing parallel flow heat exchange drying, screening, cooling and wrapping to obtain a diammonium phosphate granular product with high nitrogen content;
the parallel-flow heat exchange drying is to send ammonium phosphate materials to a dryer to perform parallel-flow heat exchange drying with hot air from a hot-blast stove at 530 ℃, gas phase in an ammoniation granulator is washed sequentially by a drying washing tower and a tail gas washing tower in the drying process, the tail gas washing tower consists of a prewashing tower and a granulation washing tower, the gas phase firstly passes through the prewashing tower and then enters the granulation washing tower, and the drying washing tower and the granulation washing tower can absorb ammonia gas and dust; the water content of the diammonium phosphate is 2.0%; in an ammoniation granulator, three ways for the ammonium phosphate material to become a diammonium phosphate granular product are coating, bonding and self-granulation, wherein the coating granulation has the best appearance quality; the screening is carried out by four stages; the cooling is to send the screened qualified materials into a fluidized bed through a chute, and then to drive the materials to float and cool by cooling air; and the coating is to send the cooled material into a coating machine through an elephant trunk, then uniformly coat the material with coating oil, and send the material into a finished product belt through the elephant trunk, wherein the mass ratio of the diammonium phosphate to the coating oil is 500:1.0 during the coating.
Further, in the first step and the second step, the neutralization degree of the first neutralization reaction between the phosphoric acid and the liquid ammonia is 1.515; the neutralization degree of the second neutralization reaction is 1.88, and the water content of the ammonium phosphate material is 3.45%.
As shown in fig. 1, 2 and 3, the ammoniation granulator for increasing the nitrogen content of a 64% diammonium phosphate product comprises a return port 1, a tubular reactor 2, a baffle 3, a cylinder 4, a gas phase outlet 5, a baffle door 6, a baffle discharge port 7, a baffle door movable observation port 8 and a particle feed port 9, wherein the baffle 3 is provided with a baffle vent 10, the return port 1 is provided with a return port vent 11, and the return port vent 11 is directly connected with the return port 1; the axial flow fan 12 is arranged close to the return port ventilation opening 11, and the axial flow fan 12 is connected with the return port 1 through the return port ventilation opening 11; only two movable observation ports 8 are arranged; the baffle vent 10 is close to the tubular reactor 2 and remote from the baffle discharge opening 7.
Comparative example 1
The differences from the embodiments 1 to 5 are as follows: the granulator is a traditional ammoniation granulator, the structure of the ammoniation granulator is shown in figures 4, 5 and 6, the ammoniation granulator comprises a material return port 1, a tubular reactor 2, a baffle 3, a barrel 4, a gas phase outlet 5, a baffle door 6, a baffle discharge port 7, a baffle door movable observation port 8 and a particle feed port 9, the number of the baffle door movable observation ports 8 is six, and other conditions are unchanged.
Comparative example 2
The differences from the embodiments 1 to 5 are as follows: in the preparation of diammonium phosphate, the procedure was carried out according to the examples in patent application CN201910589537.9, with the other conditions being unchanged.
Comparative example 3
The differences from the embodiments 1 to 5 are as follows: in the preparation of diammonium phosphate, the procedure was carried out according to the examples in patent application CN201910144697.2, with the other conditions being unchanged.
Comparative example 4
The differences from the embodiments 1 to 5 are as follows: when granulating, the ammoniation granulator is the ammoniation device of the diammonium phosphate granulator disclosed in patent application CN201620722669.6, and other conditions are not changed.
Comparative example 5
The differences from the embodiments 1 to 5 are as follows: in the granulation, the ammoniation granulator used was the granulator with double tube reactor as given in patent application CN201510184100.9, the other conditions being unchanged.
To further illustrate that the present invention can achieve the technical effects, the following experiments were performed:
the method of examples 1 to 5 and comparative examples 1 to 5 of the present application was used to prepare diammonium phosphate, and the experimental results are shown in table 1 below.
TABLE 1
| Group of | N content in diammonium phosphate | Degree of neutralization by prewashing | Degree of reverse tube neutralization | Neutralization degree of secondary ammoniation |
| Example 1 | 18.9％ | 0.37 | 1.510 | 1.870 |
| Example 2 | 19.1％ | 0.35 | 1.520 | 1.850 |
| Example 3 | 18.7％ | 0.33 | 1.510 | 1.860 |
| Example 4 | 18.8％ | 0.38 | 1.530 | 1.880 |
| Example 5 | 19.3％ | 0.32 | 1.500 | 1.900 |
| Comparative example 1 | 16.2％ | 0.73 | 1.460 | 1.470 |
| Comparative example 2 | 17.3％ | 0.68 | 1.450 | 1.460 |
| Comparative example 3 | 17.4％ | 0.66 | 1.440 | 1.450 |
| Comparative example 4 | 15.6％ | 0.78 | 1.420 | 1.430 |
| Comparative example 5 | 15.1％ | 0.76 | 1.430 | 1.440 |
As can be seen from the experimental data in Table 1, compared with the prior art, the production method of diammonium phosphate and the ammonification granulator can improve the nitrogen content of the product, reduce the degree of neutralization in prewashing (the degree of neutralization is less than 0.45), stably control the degree of neutralization in pipe reverse neutralization (the degree of neutralization in pipe reverse neutralization is 1.500-1.530), increase the degree of neutralization in secondary ammonification (the degree of neutralization in secondary ammonification is 1.85-1.90), improve the content of N in 64% diammonium phosphate products (the content of N in diammonium phosphate products is more than 17.80%), and in the production process, the ammonification granulator is not easy to have the phenomena of pipe reverse blocking, granulator running rarefaction, material agglomeration and the like, and the start-up rate is improved.
In summary, the method has the advantages that the production process of diammonium phosphate is creatively improved, the problem of gas phase short circuit in the granulator is solved, the concentration of water vapor in the granulator is reduced, the degree of neutralization in prewashing is reduced (the degree of neutralization is less than 0.45), the degree of neutralization in tube reaction is stably controlled (the degree of neutralization in tube reaction is 1.500-1.530), the degree of neutralization in secondary ammoniation is increased (the degree of neutralization in secondary ammoniation is 1.85-1.90), and the content of N in 64% diammonium phosphate products is increased; the N content of 64 percent diammonium phosphate products produced by the ammoniation granulator is more than 17.80 percent, the water content is reduced, the requirement of various complex component source acid indexes can be met, the phenomena of pipe reverse blocking, granulator dilution running, material agglomeration and the like are effectively restrained, and the start-up rate is improved; to prior art's shortcoming, carry out technical transformation to the ammoniation granulator, close four activity shutter viewing apertures in ammoniation granulator shutter top, stop the gaseous phase short circuit, in addition, add the blow vent at ammoniation granulator baffle, add vent and axial fan at ammoniation granulator returning charge mouth, reduce the interior steam enrichment of ammoniation granulator cavity, increase the gaseous phase and flow, ensure the interior micro-negative pressure state of ammoniation granulator simultaneously, stop the ammonia and escape, cause ammonia loss and safe environmental protection risk.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (10)
1. The production method for increasing the nitrogen content of 64% diammonium phosphate is characterized by comprising the following steps:
step one, a pipe reverse pump sends phosphoric acid in a pipe reverse tank to a mixer to perform a first neutralization reaction with liquid ammonia to obtain slurry;
uniformly spraying the slurry into an ammoniation granulator, and performing secondary neutralization reaction on the slurry and liquid ammonia fed by an ammonia distributor to obtain an ammonium phosphate material;
and step three, after the ammonium phosphate material is granulated in an ammoniation granulator, performing parallel flow heat exchange drying, screening, cooling and wrapping to obtain a diammonium phosphate particle product with high nitrogen content.
2. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: in step one, P in the phosphoric acid2O5The content is 39-41%.
3. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: in the first step and the second step, the neutralization degree of the first neutralization reaction between the phosphoric acid and the liquid ammonia is 1.500-1.530; the neutralization degree of the second neutralization reaction is 1.85-1.90, and the water content of the ammonium phosphate material is 3.2% -3.65%.
4. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: and step three, the parallel-flow heat exchange drying is to send the ammonium phosphate material to a drying machine to perform parallel-flow heat exchange drying with hot air from a hot-blast stove at 500-550 ℃, a gas phase in an ammoniation granulator is washed sequentially by a drying washing tower and a tail gas washing tower in the drying process, the tail gas washing tower consists of a pre-washing tower and a granulation washing tower, the gas phase firstly passes through the pre-washing tower and then enters the granulation washing tower, and the drying washing tower and the granulation washing tower can absorb ammonia gas and dust.
5. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: in the third step, the water content of the diammonium phosphate is 1.8% -2.5%.
6. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: in step three, in the ammoniation granulator, three ways of changing the ammonium phosphate material into the diammonium phosphate granular product are coating, bonding and self-granulation.
7. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: in step three, the screening is performed by four stages.
8. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: and step three, the cooling is to send the screened qualified materials into a fluidized bed through a chute, and then the materials are driven by cooling air to float and cool.
9. The production method for increasing the nitrogen content of 64% diammonium phosphate according to claim 1, characterized in that: and step three, the cooled material is conveyed into a wrapping machine through a chute, then is uniformly wrapped by wrapping oil, and is conveyed into a finished product belt through the chute, wherein the mass ratio of the diammonium phosphate to the wrapping oil is 500: 0.9-1.2 during wrapping.
10. An ammoniation granulator for improving the nitrogen content of 64% diammonium phosphate products is characterized in that: the ammonification granulator comprises a return port (1), a tubular reactor (2), a baffle (3), a barrel (4), a gas phase outlet (5), a baffle door (6), a baffle discharge port (7), a baffle door movable observation port (8) and a particle feed port (9), wherein a baffle vent (10) is arranged on the baffle (3), a return port vent (11) is arranged on the return port (1), and the return port vent (11) is directly connected with the return port (1); the axial flow fan (12) is arranged close to the return port ventilation opening (11), and the axial flow fan (12) is connected with the return port (1) through the return port ventilation opening (11); the number of the movable observation ports (8) of the stop door is only two; the baffle vent (10) is close to the tubular reactor (2) and is far away from the baffle discharge hole (7).
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| CN111423272A (en) * | 2020-03-31 | 2020-07-17 | 湖北万丰化工有限公司 | Method for producing fertilizer by slurry method |
| CN114560453A (en) * | 2022-03-24 | 2022-05-31 | 内蒙古大地云天化工有限公司 | Preparation method of diammonium phosphate |
| CN114988967A (en) * | 2022-06-13 | 2022-09-02 | 贵州开磷集团股份有限公司 | Preparation method of compound fertilizer added with zinc element |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111423272A (en) * | 2020-03-31 | 2020-07-17 | 湖北万丰化工有限公司 | Method for producing fertilizer by slurry method |
| CN114560453A (en) * | 2022-03-24 | 2022-05-31 | 内蒙古大地云天化工有限公司 | Preparation method of diammonium phosphate |
| CN114988967A (en) * | 2022-06-13 | 2022-09-02 | 贵州开磷集团股份有限公司 | Preparation method of compound fertilizer added with zinc element |
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