CN103303887B - Method for producing high-nutrient monoammonium phosphate by dual-tube reverse process - Google Patents
Method for producing high-nutrient monoammonium phosphate by dual-tube reverse process Download PDFInfo
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- CN103303887B CN103303887B CN201310201747.9A CN201310201747A CN103303887B CN 103303887 B CN103303887 B CN 103303887B CN 201310201747 A CN201310201747 A CN 201310201747A CN 103303887 B CN103303887 B CN 103303887B
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Abstract
The invention discloses a method for producing high-nutrient monoammonium phosphate by a dual-tube reverse process. The method adopts wet-process phosphoric acid and liquid ammonia as raw materials and performs fast replacement on diammonium phosphate and produces chemical fertilizer-level high-nutrient monoammonium phosphate, and comprises the following steps of: production preparation: reducing solid content in strong phosphoric acid; earlier stage of production: keeping the equipment running in a low-load state, and performing single-tube revertive control to gradually transit to a monoammonium phosphate production process; and production process: entering a stable control stage of the production process, producing with a dual-tube reverse process, and adding certain amount of secondary ammonia supplement into a material bed of a granulator as necessary. By adopting the method disclosed by the invention, the total nutrient of the monoammonium phosphate product reaches 63%, the equipment runs stably, the yield can reach 45-70t/h, the contents of ammonia, phosphorus and potassium in the product are 11, 52 and 0 respectively, the water content is low, and a few impurities are contained; and the product is a water-soluble binary quick-acting compound fertilizer, is widely applied to agricultural production and can be used as a main raw material for preparing a nitrogen-phosphorus-potassium ternary compound fertilizer.
Description
Technical field
The present invention relates to phosphorus ammonium, specifically a kind of method adopting two-tube anti-explained hereafter height nutrient monoammonium phosphate.
Technical background
Current, domestic ammonium phosphate product market is seriously saturated, Improving The Quality of Products, the breakthrough and innovation realizing product is the important channel of enterprise competitive power, promote that product diversification is with the demand of satisfied different client, be enterprise in the market competition of fierceness, base oneself upon market, strengthen the important leverage of the enterprise ability to ward off risks.Diammonium phosphate device realizing quick switching and the stably manufactured of monoammonium phosphate technique, the batch production of especially high nutrient monoammonium phosphate, is explore the profound level of production equipment function diversification.
Through retrieval, in Chinese patent database, not yet occur that utilizing phosphoric acid by wet process to adopt on diammonium phosphate device in two-tube anti-technique realizes high nutrient monoammonium phosphate production methods involving at present.
Summary of the invention
The object of this invention is to provide a kind of method, be adopt phosphoric acid by wet process and liquefied ammonia to be raw material, switch fast in diammonium phosphate and produce the high nutrient monoammonium phosphate of agriculture level (NH
4h
2pO
4, MAP), realize the multifunction of production equipment.
provided by the inventionthe method of two-tube anti-explained hereafter height nutrient monoammonium phosphate is adopted to comprise the steps:
(1)
operational preparation
By two water wet method dilute phosphoric acids through pump circulation vacuum evaporation, form concentration 48%P
2o
5strong phosphoric acid enters clarifying tank and carries out sedimentation clarification, and removing suspended solid wherein, reduces solid content in strong phosphoric acid.
Raw material strong phosphoric acid and liquefied ammonia stock abundance.
(2) to change the line of production process
Before changing the line of production, system returning charge amount is dropped to about 380t, changes the line of production in process, adopt single tube revertive control, gradually to the transition of monoammonium phosphate production technique, simultaneity factor master batch (original state is diammonium phosphate returning charge) is replaced by monoammonium phosphate comprehensively.
From the strong phosphoric acid (P of strong phosphoric acid clarification storage tank
2o
5content 48%) flow 95% switches and enters tubular reactor complex acid groove, holding tube anti-complex acid groove buffering Liquid level 60%, tubular reactor complex acid density 1.56 ~ 1.60g/cm
3; Concentration about 45 ~ 48%, after another part flow 5% strong phosphoric acid then enters ammonia scrubber circulation cleaning tail gas generated by granulation, washings pond for recovering is back to by trench, be mixed together from the washings of each washing tower and liquid seal trough thereof with backflow, supplement the dilution of certain process water simultaneously, under agitator effect, keep Homogeneous phase mixing, be delivered to each washing tower liquid seal trough again and circulation cleaning is carried out to tail gas such as granulation, drying, cooling, equipment dedustings.
The whitewashing of one of them tubular reactor is stopped to run, single pipe reactor is kept to run to monoammonium phosphate process transition, the tubular reactor degree of neutralization (N/P) of on-line operation is set between 0.6 ~ 0.8, the set(ting)value granulation of degree of neutralization (N/P), according to granulation material condition selecting, is cancelled simultaneously and add secondary benefit ammonia in tablets press, the feeding coal reacted due to phosphoric acid and liquefied ammonia is nonlinear relationship, for suppressing the disturbance occurring that the violent amplitude of change is larger, overcome the delayed of controlled process, we are by parametric controller DCS (Distributed control system, distributed control system) with phosphoric acid flow for master loop, with liquefied ammonia flow for subloop, adopt serials control, phosphoric acid feed proportioning controller according to the output phosphoric acid flow of master loop setter as the set-point of subloop setter liquefied ammonia, implement phosphoric acid and liquefied ammonia delivery rate servo antrol, namely after phosphoric acid flow determines output, liquefied ammonia delivery rate formula is stored in DCS control, degree of neutralization (N/P) is artificial set(ting)value, Controlling System is in conjunction with degree of neutralization set(ting)value and current phosphoric acid feed flow flow, automatic calculating regulator solution ammonia flow, and export flows of liquid ammonia amount controller to, following relational expression stores in dcs, in order to calculate the delivery rate of liquefied ammonia:
In formula, SO
4 2-refer to sulfuric acid amount remaining in phosphoric acid, with P
2o
5supply be directly proportional.
Tubular reactor steady running; intrasystem returning charge (diammonium phosphate) replaced by monoammonium phosphate material gradually that produce; in the process; analysis and Control is carried out to tablets press product material; when its material pH value drops to 4.8; system returning charge replace by monoammonium phosphate material, show that material transitioning processes completes.
(3) production process controls
Transition material all replaced complete after, start to produce the stability contorting stage entering production technique, keep raw material phosphoric acid flow to enter tubular reactor complex acid groove and ammonia scrubber ratio (95:5) is constant; The tubular reactor degree of neutralization of on-line operation is set to 0.8 ~ 0.88; the whitewashing of simultaneously opening another tubular reactor is produced; degree of neutralization is similarly 0.80 ~ 0.88; by video monitoring and field observation tablets press ammoniation and granulation state and the dry wet situation of tablets press product material; the whitewashing amount of dynamic adjustments two tubular reactors and degree of neutralization, the whitewashing flow of two tubular reactors amounts to 45 ~ 60m
3/ h, adds certain secondary at tablets press material bed if desired and mends ammonia, granulation material degree of neutralization is brought up to 0.95 ~ 1.05 further, to keep tablets press outlet material to be granular dispersion state, and tablets press product material pH ≈ 4.8;
Enter the fresh clarification strong phosphoric acid of employing and the washings mixed preparing of tubular reactor complex acid groove, keep its density p (H
3pO
4)=1.56 ~ 1.60g/cm
3, in tubular reactor complex acid groove, add the tinting material of respective numbers simultaneously, the phosphoric acid prepared gives sour pump pressure-increasing unit through two tubular reactors, sentence vertical direction with the high-pressure liquid ammonia from liquefied ammonia tank field at the mixing head of two tubular reactors respectively to cut, there is the reaction of violent acid-base neutralisation immediately, generate High Temperature High Pressure (T=110 DEG C ~ 135 DEG C, P=0.38MPa ~ 0.55Mpa) phosphor ammonium slurry, tablets press is entered by tubular reactor slip distribution pipe, be ejected on the returning charge material bed of rotary drum granulator by means of pressure itself, returning charge is than about 4.5 ~ 6.5:1, dry wet stock is with coating, bonding, granulation is completed from modes such as granulating, the heat simultaneously relying on reaction to generate completes moisture evaporation, form the granule materials of dispersion.
Granulation material leaves tablets press, tied chute enter rotary dryer by means of its action of gravity, carries out and fluidized drying with the high-temperature flue gas from hotblast stove, and drying machine is tiny structure under dried tail gas fan action.
Drying machine product material through electro-magnet except magnetic and drying machine product belt, dried material are through the conveying of bucket elevator; under material distributing valve effect; material is uniformly distributed to five large grain sieve apparatus; large grain sifted material loading; enter after crusher carries out fragmentation; all collected by return collecting belt, promote conveying through returning charge bucket elevator subsequently, return tablets press and carry out granulation again.
The blanking of large grain sifted enters Liang Tai respectively enter finished product screen extension set through chute and the conveying of finished product bucket elevator, finished product screen blanking collected by return collecting belt, the granulation again of returning charge tablets press.
Finished product screen extension set extracts on-the-sieve material particle as diammonium phosphate product through cooling bed air blast cooling, dedusting, to be promoted by product bucket elevator and sub-material enters two product sieve apparatus again carries out stricter fine work and sieve, further preferred particulates, evenly accurate to guarantee screening Granularity Distribution; Screening product out carries out external parcel through delivering into parcel cylinder to product interpolation parcel oil, and to prevent, caking from appearring in product in storage transportation, wet the phenomenons such as tide, and product wrapping enters storehouse in bulk storage packaging through Belt Conveying.
in aforesaid method, described clarifying tank strong phosphoric acid specification sees the following form 1:
| Density (g/cm 3） | P 2O 5 | F | SO 3 | Fe 2O 3 | Al 2O 3 | MgO | Solid content |
| 1.646 | 49% | 0.55% | 4.50% | 0.40% | 0.20% | 2.00% | 0.95% |
In aforesaid method, Liquid Ammonia Storage in in ammonia device buffering spherical tank, its ammonia content >=99.9%, residuals content≤0.1%, waiting when receiving production equipment for ammonia instruction, to start for ammonia pump supercharging and to production main device conveying liquefied ammonia.
In aforesaid method, the slip distribution pipe of described tubular reactor A and tubular reactor B is all arranged two nozzles, the length scale of this nozzle can regulate, for controlling the announcement of reaction time and whitewashing flow.
In aforesaid method, described tablets press wall there is ventilation breather, liner rubber plate; when tablets press rotates, when rubber plate is positioned at top and bottom, air is sucked by ventilation breather successively and discharges; promote the material of rubber plate springing except debanding, keep tablets press cleaning inside.
In aforesaid method, the inlet air flow temperature of described drying machine 350 ~ 650 DEG C, outlet air temperature 85 ~ 95 DEG C, the machine product that can keep dry material water content controls≤2.5%.
In aforesaid method, described large grain sieve apparatus is oscillatory type single-deck screen, mesh size 4mm.
In aforesaid method, described crusher is double-shaft chain hammer, and rotating speed one is fast one slow.
In aforesaid method, the mesh size 2mm of described finished product screen extension set.
In aforesaid method, the dust of described each belt conveyor, bucket elevator, sieve apparatus, crusher, cooling bed, drying machine all carries out cyclonic separation, and the dust granules separated enters return collecting belt, the granulation again of returning charge tablets press.
In aforesaid method, the tail gas produced, under fan action, enters vent gas washing system, collects washings and carries out circulation cleaning.
In aforesaid method, washing system adopts the washings of lower concentration to carry out circulated sprinkling washing to each washing tower, add certain process water to dilute simultaneously, keep concentration and the washing effect thereof of washings, be added with filler in each washing tower, increase gas liquid interfacial area, strengthening washing effect, washings is all recycled to washings pond for recovering as system water supplement, and tail gas is then discharged by chimney through blower fan draw.
Method provided by the invention has following advantage:
(1) utilize diammonium phosphate device to produce high nutrient agricultural level monoammonium phosphate, realize the multifunction of phosphorus ammonium production equipment; (2) realize monoammonium phosphate device to realize switching fast, produce the product comprising the different sizes such as monoammonium phosphate (MAP) and diammonium phosphate (DAP), expand product type, meet multi-demands, strengthen enterprise to the adaptability of turn of the market; (3) improve a kind of production method of high nutrient monoammonium phosphate, enterprise can be helped to pursue P in the age that Mineral resources are in short supply
2o
5maximizing the benefits, (4), in the face of common phosphorus ammonium market saturation situation, the monoammonium phosphate current demand of high nutrient is large, enterprise can be helped to open up a market, strive together with domestic and international quality products, improves enterprise competitiveness.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
In figure: 1-strong phosphoric acid clarifying tank; 2-manages anti-complex acid groove; 3-tablets press; 4-drying machine; 5-tubular reactor A; 6-tubular reactor B; 7-ammonia scrubber; The large grain sieve apparatus of 8-; 9-crusher; 10-tail gas washing tower; 11-washings pond for recovering; 12-finished product screen extension set; 13-cyclonic separator; 14-cooling bed; 15-chimney; 16-product sieve apparatus; 17-wraps up cylinder; 18-hotblast stove; 19-anhydrous ammonia tank; 20-gas blower; 21-stores up at storehouse of faling apart; 22-secondary capsulation cylinder.
Embodiment
The monoammonium phosphate that Wengfu phosphate fertilizer plant adopts the present invention to adopt double hose reaction formula technique to carry out high nutrient on 600kt/a diammonium phosphate device is produced, and production process parameter stability, equipment running status is good.Controlling System is the dynamo-electric DCS(distributed control system of Yokogawa) CENTUM CS parametric controller.
(1) Operational preparation
The phosphoric acid of Wengfu Group Co., Ltd. Wengfu phosphate fertilizer plant 20kt/a Wet Phosphoric Acid Plant enters strong phosphoric acid clarifying tank 1 through the strong phosphoric acid of pump circulation vacuum evaporation and carries out sedimentation clarification, removing suspended solid wherein, reduces solid content in strong phosphoric acid.
(2) to change the line of production process
System returning charge amount is dropped to about 380t, changes the line of production in process, adopt single tube revertive control, gradually to the transition of monoammonium phosphate production technique, simultaneity factor master batch (diammonium phosphate) replaced by monoammonium phosphate comprehensively.
From the strong phosphoric acid (P of strong phosphoric acid clarifying tank 1
2o
5content 48%) flow 95% switch enter pipe anti-complex acid groove 2, holding tube anti-complex acid groove 2 Liquid level 60%, tubular reactor complex acid density 1.56 ~ 1.60g/cm
3; After another part flow 5% strong phosphoric acid then enters ammonia scrubber 7 circulation cleaning tail gas generated by granulation, washings pond for recovering 11 is back to by trench, be mixed together from the washings of each washing tower and liquid seal trough thereof with backflow, supplement the dilution of certain process water simultaneously, under agitator effect, keep Homogeneous phase mixing, be delivered to each washing tower liquid seal trough again and circulation cleaning is carried out to tail gas such as granulation, drying, cooling, equipment dedustings.
The whitewashing of tubular reactor A5 is stopped to run, keep tubular type reactor B 6 run transition, be set between 0.6 ~ 0.8 by tubular reactor B6 degree of neutralization (N/P), the set(ting)value granulation of degree of neutralization (N/P), according to granulation material condition selecting, is cancelled simultaneously and add secondary benefit ammonia in tablets press, by parametric controller DCS (Distributed control system, distributed control system) with phosphoric acid flow for master loop, with liquefied ammonia flow for subloop, adopt serials control, phosphoric acid feed proportioning controller according to the output phosphoric acid flow of master loop setter as the set-point of subloop setter liquefied ammonia, implement phosphoric acid and liquefied ammonia delivery rate servo antrol, namely after phosphoric acid flow determines output, liquefied ammonia delivery rate formula is stored in DCS control, degree of neutralization (N/P) is artificial set(ting)value, Controlling System combines according to formula, degree of neutralization set(ting)value and current phosphoric acid feed flow flow, automatic calculating regulator solution ammonia flow, and export flows of liquid ammonia amount controller to, following relational expression stores in dcs, in order to calculate the delivery rate of liquefied ammonia:
In formula, SO
4 2-refer to sulfuric acid amount remaining in phosphoric acid, with P
2o
5supply be directly proportional;
Tubular reactor B6 steady running, intrasystem returning charge (diammonium phosphate) replaced by monoammonium phosphate material gradually that produce, in the process, analysis and Control is carried out to tablets press 3 material of producing, when its material pH value drops to 4.8, system returning charge replace by monoammonium phosphate material, show that material transitioning processes completes;
(3) production process controls
Transition material all replaced complete after, start to produce the stability contorting stage entering production technique, keep raw material phosphoric acid flow to enter tubular reactor complex acid groove 2 and ammonia scrubber 7 ratio (95:5) is constant; Tubular reactor B6 degree of neutralization is set to 0.8 ~ 0.88; the whitewashing of simultaneously opening tubular type reactor A 5 is produced; degree of neutralization is similarly 0.80 ~ 0.88; to be produced the dry wet situation of material by video monitoring and field observation tablets press ammoniation and granulation state and tablets press 3; the whitewashing amount of dynamic adjustments two tubular reactors and degree of neutralization, the whitewashing flow of two tubular reactors amounts to 45 ~ 60m
3/ h, adds certain secondary at tablets press material bed if desired and mends ammonia, granulation material degree of neutralization is brought up to 0.95 ~ 1.05 further, and to keep tablets press 3 outlet material to be granular dispersion state, tablets press 3 is produced material pH ≈ 4.8;
Enter the fresh clarification strong phosphoric acid of employing and washings mixed preparing of managing anti-complex acid groove 2, keep its density p (H
3pO
4)=1.56 ~ 1.60g/cm
3, in the anti-complex acid groove 2 of pipe, add the tinting material of respective numbers simultaneously, the phosphoric acid prepared gives sour pump pressure-increasing unit through two tubular reactors, sentence vertical direction with the high-pressure liquid ammonia from anhydrous ammonia tank 19 at the mixing head of two tubular reactors respectively to cut, there is the reaction of violent acid-base neutralisation immediately, generate High Temperature High Pressure (T=110 DEG C ~ 135 DEG C, P=0.38MPa ~ 0.55Mpa) phosphor ammonium slurry, tablets press 3 is entered by tubular reactor slip distribution pipe, be ejected on the returning charge material bed of rotary drum granulator by means of pressure itself, returning charge is than about 4.5 ~ 6.5:1, dry wet stock is with coating, bonding, granulation is completed from modes such as granulating, the heat simultaneously relying on reaction to generate completes moisture evaporation, form the granule materials of dispersion.
Granulation material leaves tablets press 3, tied chute enter rotary dryer 4 by means of its action of gravity, carries out and fluidized drying with the high-temperature flue gas from hotblast stove 18, and drying machine 4 is tiny structure under dried tail gas fan action;
Drying machine 4 produces material through electro-magnet except magnetic and drying machine product belt, dried material are through the conveying of bucket elevator; under material distributing valve effect; material is uniformly distributed to five large grain sieve apparatus 8; the oversize of large grain sieve apparatus 8 enters after crusher 9 carries out fragmentation; all collected by return collecting belt; promote conveying through returning charge bucket elevator subsequently, return tablets press 3 and carry out granulation again.
The blanking of large grain sifted 8 enters Liang Tai respectively through chute and the conveying of finished product bucket elevator and enters finished product screen extension set, finished product screen blanking collected by return collecting belt, the granulation again of returning charge tablets press.
Finished product screen extension set extracts on-the-sieve material particle as diammonium phosphate product through cooling bed 14 air blast cooling, dedusting, to be promoted by product bucket elevator and sub-material enters two product sieve apparatus 16 again carries out stricter fine work and sieve, further preferred particulates, evenly accurate to guarantee screening Granularity Distribution; Screening product out carries out external parcel through delivering into parcel cylinder 17 pairs of products interpolation parcel oil, and to prevent, caking from appearring in product in storage transportation, wet the phenomenons such as tide, and product wrapping enters storehouse in bulk storage packaging through Belt Conveying.
in aforesaid method, described clarifying tank strong phosphoric acid specification sees the following form 1:
| Density (g/cm 3） | P 2O 5 | F | SO 3 | Fe 2O 3 | Al 2O 3 | MgO | Solid content |
| 1.646 | 49% | 0.55% | 4.50% | 0.40% | 0.20% | 2.00% | 0.95% |
In aforesaid method, Liquid Ammonia Storage in in ammonia device buffering spherical tank, its ammonia content >=99.9%, residuals content≤0.1%, waiting when receiving production equipment for ammonia instruction, to start for ammonia pump supercharging and to production main device conveying liquefied ammonia.
In aforesaid method, the slip distribution pipe of described tubular reactor A5 and tubular reactor B6 is all arranged two nozzles, the length scale of this nozzle can regulate.
In aforesaid method, described tablets press 3 wall there is ventilation breather, liner rubber plate; when tablets press 3 rotates, when rubber plate is positioned at top and bottom, air is sucked by ventilation breather successively and discharges; promote the material of rubber plate springing except debanding, keep tablets press 3 cleaning inside.
In aforesaid method, the inlet air flow temperature of described drying machine 4 350 ~ 650 DEG C, outlet air temperature 85 ~ 95 DEG C, the machine 4 that can keep dry produce material water content control≤2.5%.
In aforesaid method, described large grain sieve apparatus 8 is oscillatory type single-deck screen, mesh size 4mm.
In aforesaid method, described crusher 9 is double-shaft chain hammer, and rotating speed one is fast one slow.
In aforesaid method, the mesh size 2mm of described finished product screen extension set 12.
In aforesaid method, the dust of described each belt conveyor, bucket elevator, sieve apparatus, crusher, cooling bed, drying machine all carries out cyclonic separation, and the dust granules separated enters return collecting belt, the granulation again of returning charge tablets press.
In aforesaid method, the tail gas produced, under fan action, enters vent gas washing system, collects washings and carries out circulation cleaning.
In aforesaid method, washing system adopts the washings of lower concentration to carry out circulated sprinkling washing to each washing tower, add certain process water to dilute simultaneously, keep concentration and the washing effect thereof of washings, be added with filler in each washing tower, increase gas liquid interfacial area, strengthening washing effect, washings is all recycled to washings pond for recovering as system water supplement, and tail gas is then discharged by chimney through blower fan draw.
Use aforesaid method to produce high nutrient monoammonium phosphate, product highly water-soluble, do not lump, stable in properties in atmosphere, its PH ≈ 4.5 is a kind of efficient compound fertilizers being rich in N, P binary effective element, total nutrient (P
2o
5+ N) reach 63%, wherein available phosphorus (P
2o
5) content is greater than 52%, nitrogen (N) content is greater than 12%, is the high-quality basic material of preparation N, P, K ternary compound fertilizer, also be adapted at plant growth stage plant fertilizer and foliage-spray used, be conducive to growth and the growth of plant root, good water solubility, fertilizer efficiency period is long.
table 3: high nutrient monoammonium phosphate specification
| Total nutrient | Available phosphorus | Water-soluble phosphorus | Nitrogen | Moisture content | Granularity (2-4mm) | Intensity |
| 63% | 52.3% | 51.0% | 11.0% | 1.2% | 94% | 45N |
Claims (10)
1. adopt a method for two-tube anti-explained hereafter height nutrient monoammonium phosphate, it is characterized in that the method comprises following steps:
(1) Operational preparation
Be strong phosphoric acid and send into strong phosphoric acid clarifying tank (1) to carry out sedimentation clarification through pump circulation vacuum evaporation by the phosphoric acid of Wet Phosphoric Acid Plant, removing suspended solid wherein, reduces solid content in strong phosphoric acid;
(2) to change the line of production process
System returning charge amount is dropped to about 380t, changes the line of production in process, adopt single tube revertive control, gradually to the transition of monoammonium phosphate production technique, simultaneity factor master batch and diammonium phosphate, replaced by monoammonium phosphate comprehensively;
From the strong phosphoric acid of strong phosphoric acid clarifying tank (1), its P
2o
5content 48%, flow 95% switch enter pipe anti-complex acid groove (2), holding tube anti-complex acid groove (2) Liquid level 60%, tubular reactor complex acid density 1.56 ~ 1.60g/cm
3; After another part flow 5% strong phosphoric acid then enters ammonia scrubber (7) circulation cleaning tail gas generated by granulation, washings pond for recovering (11) is back to by trench, be mixed together from the washings of each washing tower and liquid seal trough thereof with backflow, supplement the dilution of certain process water simultaneously, under agitator effect, keep Homogeneous phase mixing, be delivered to each washing tower liquid seal trough again and circulation cleaning is carried out to granulation, drying, cooling, equipment dedusting tail gas;
Stop tubular reactor A(5) whitewashing run, keep tubular type reactor B (6) run transition, by tubular reactor B(6) degree of neutralization (N/P) is set between 0.6 ~ 0.8, the set(ting)value of degree of neutralization (N/P), according to granulation material condition selecting, is cancelled simultaneously and add secondary benefit ammonia in tablets press, by parametric controller DCS with phosphoric acid flow for master loop, with liquefied ammonia flow for subloop, adopt serials control, phosphoric acid feed proportioning controller according to the output phosphoric acid flow of master loop setter as the set-point of subloop setter liquefied ammonia, implement phosphoric acid and liquefied ammonia delivery rate servo antrol, namely after phosphoric acid flow determines output, liquefied ammonia delivery rate formula is stored in DCS control, degree of neutralization (N/P) is artificial set(ting)value, Controlling System is in conjunction with degree of neutralization set(ting)value and current phosphoric acid feed flow, DCS Controlling System is in conjunction with delivery rate formula and degree of neutralization (N/P) set(ting)value and current phosphoric acid flow, automatic calculating regulator solution ammonia flow, and export flows of liquid ammonia amount controller to, following relational expression stores in dcs, in order to calculate the delivery rate of liquefied ammonia:
In formula, SO
4 2-refer to sulfuric acid amount remaining in phosphoric acid, with P
2o
5supply be directly proportional; Tubular reactor B(6) steady running, intrasystem returning charge replaced by monoammonium phosphate material gradually that produce, in the process, analysis and Control is carried out to tablets press (3) product material, when its material pH value drops to 4.8, system returning charge replace by monoammonium phosphate material, show that material transitioning processes completes;
(3) production process controls
Transition material all replaced complete after, start to produce the stability contorting stage entering production technique, keep raw material phosphoric acid flow to enter tubular reactor complex acid groove (2) and ammonia scrubber (7) constant rate; By tubular reactor B(6) degree of neutralization is set to 0.8 ~ 0.88; the whitewashing of simultaneously opening tubular type reactor A (5) is produced; degree of neutralization is similarly 0.80 ~ 0.88; by video monitoring and field observation tablets press ammoniation and granulation state and the dry wet situation of tablets press (3) product material; the whitewashing amount of dynamic adjustments two tubular reactors and degree of neutralization, the whitewashing flow of two tubular reactors reaches 45 ~ 60m
3/ h, adds certain secondary at tablets press material bed if desired and mends ammonia, granulation material degree of neutralization is brought up to 0.95 ~ 1.05 further, to keep tablets press (3) outlet material to be granular dispersion state, and tablets press (3) product material pH ≈ 4.8;
Enter the material of managing anti-complex acid groove (2) and adopt fresh clarification strong phosphoric acid and washings mixed preparing, keep its density p (H
3pO
4)=1.56 ~ 1.60, in the anti-complex acid groove (2) of pipe, add the tinting material of respective numbers simultaneously, the phosphoric acid prepared gives sour pump pressure-increasing unit through two tubular reactors, sentence vertical direction with the high-pressure liquid ammonia from anhydrous ammonia tank (19) at the mixing head of two tubular reactors respectively to cut, there is the reaction of violent acid-base neutralisation immediately, generate the phosphor ammonium slurry of High Temperature High Pressure, tablets press (3) is entered by tubular reactor slip distribution pipe, be ejected on the returning charge material bed of rotary drum granulator by means of pressure itself, returning charge is than 4.5 ~ 6.5:1, dry wet stock is with coating, bonding, granulation is completed from granulating mode, the heat simultaneously relying on reaction to generate completes moisture evaporation, form the granule materials of dispersion,
Granulation material leaves tablets press (3), enters rotary dryer (4) by means of its action of gravity through chute, carries out and fluidized drying with the high-temperature flue gas from hotblast stove (18), and drying machine (4) is tiny structure under dried tail gas fan action;
Drying machine (4) product material through electro-magnet except magnetic and drying machine outlet belt, bucket elevator conveying, under material distributing valve effect, material is uniformly distributed to five large grain sieve apparatus (8), the oversize of large grain sieve apparatus (8) enters after crusher (9) carries out fragmentation, all collected by return collecting belt, promote conveying through returning charge bucket elevator subsequently, return tablets press (3) and carry out granulation again;
The minus mesh of large grain sieve apparatus (8) enters two finished product screen extension sets (12) respectively through chute and the conveying of finished product bucket elevator, the minus mesh of finished product screen extension set (12) collected by return collecting belt, the granulation again of returning charge tablets press;
Finished product screen extension set (12) extracts on-the-sieve material particle as diammonium phosphate product through cooling bed (14) air blast cooling, dedusting, to be promoted by product bucket elevator and sub-material enters two product sieve apparatus (16) again carries out stricter fine work and sieve, further preferred particulates, evenly accurate to guarantee screening Granularity Distribution; Screening product out carries out external parcel through delivering into parcel cylinder (17) to product interpolation parcel oil, and to prevent, caking from appearring in product in storage transportation, wet damp phenomenon, and product wrapping enters storehouse in bulk storage packaging through Belt Conveying.
2. the method for claim 1, is characterized in that the strong phosphoric acid specification in described strong phosphoric acid clarifying tank sees the following form 1:
。
3. the method for claim 1, it is characterized in that described Liquid Ammonia Storage is in cushioning in spherical tank for ammonia device, its ammonia content >=99.9%, residuals content≤0.1%, waiting when receiving production equipment for ammonia instruction, to start for ammonia pump supercharging and to production main device conveying liquefied ammonia.
4. the method for claim 1, is characterized in that described tubular reactor A(5) and tubular reactor B(6) slip distribution pipe on two nozzles are all set, the length scale of this nozzle can regulate.
5. the method for claim 1; it is characterized in that described tablets press (3) wall has ventilation breather; liner rubber plate; when tablets press (3) rotates; when rubber plate is positioned at top and bottom; air is sucked by ventilation breather successively and discharges, and promotes the material of rubber plate springing except debanding, keeps tablets press (3) cleaning inside.
6. the method for claim 1, is characterized in that the inlet air flow temperature 350 ~ 650 DEG C of described drying machine (4), outlet air temperature 85 ~ 95 DEG C, and machine (4) the product material water content that can keep dry controls≤2.5%.
7. the method for claim 1, is characterized in that described large grain sieve apparatus (8) is oscillatory type single-deck screen, mesh size 4mm; The mesh size 2mm of described finished product screen extension set (12).
8. the method for claim 1, is characterized in that described crusher (9) is for double-shaft chain hammer, and rotating speed one is fast one slow.
9. the method for claim 1; it is characterized in that in described method; the dust of each belt, bucket elevator, sieve apparatus, crusher, cooling bed, drying machine all carries out cyclonic separation, and the dust granules separated enters return collecting belt, the granulation again of returning charge tablets press.
10. the method for claim 1, is characterized in that, in described method, the tail gas produced, under fan action, enters vent gas washing system, collects washings and carries out circulation cleaning; Washing system adopts the washings of lower concentration to carry out circulated sprinkling washing to each washing tower, add certain process water to dilute simultaneously, keep concentration and the washing effect thereof of washings, filler is added with in each washing tower, increase gas liquid interfacial area, strengthening washing effect, washings is all recycled to washings pond for recovering as system water supplement, and tail gas is then discharged by chimney through blower fan draw.
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| JP6268054B2 (en) * | 2014-07-09 | 2018-01-24 | 株式会社アナック | Method and apparatus for producing fertilizer by treating phosphoric acid mixed acid waste liquid |
| CN104529559A (en) * | 2014-12-25 | 2015-04-22 | 瓮福（集团）有限责任公司 | Device and method for increasing nitrogen content of diammonium phosphate by virtue of dual-tube reverse production process by adding urea |
| CN106831053B (en) * | 2017-02-10 | 2021-01-19 | 云南三环中化化肥有限公司 | Production method of granular and function-enhanced magnesium-containing ammonium phosphate |
| CN108314503A (en) * | 2018-05-03 | 2018-07-24 | 武汉环绿时代生态园林工程有限公司 | A kind of production system and production method of water soluble composite fertilizer |
| CN109384208A (en) * | 2018-12-20 | 2019-02-26 | 湖北六国化工股份有限公司 | A kind of the step application method and system of phosphor ammonium slurry |
| CN110590409A (en) * | 2019-09-27 | 2019-12-20 | 瓮福达州化工有限责任公司 | System and process for preparing phosphate fertilizer from raffinate |
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| CN102674282B (en) * | 2012-05-16 | 2014-08-20 | 瓮福（集团）有限责任公司 | Method for producing granular monoammonium phosphate |
| CN102689883B (en) * | 2012-06-19 | 2014-02-26 | 瓮福（集团）有限责任公司 | Method for producing diammonium phosphate from recycled phosphorus-containing filter residues |
| CN103011112A (en) * | 2012-12-12 | 2013-04-03 | 瓮福（集团）有限责任公司 | Production method of diammonium phosphate product |
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