CN1651359A - Production method of urocomposite fertilizer - Google Patents
Production method of urocomposite fertilizer Download PDFInfo
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Abstract
A urine-based composite fertilizer is prepared through reaction between urea, sulfuric and water to generate the solution of urea sulfate, adding it along with ammonia gas and basic NPK fertilizer to granulating machine, neutralizing reacting while granulating, drying, sieving, and cooling. Its advantage is low content of biuret.
Description
Technical field
The present invention relates to a kind of production method of compound manure, more precisely relate to a kind of production method of urea-base compound fertilizer.
Background technology
Urea is as the present the highest solid fertilizer of nitrogen content; be applied to farm crop for a long time; but for a long time, because urea special nature comparatively, during with the common granulation production of other base fertilizers composite fertilizer; the easy moisture absorption of product; bring difficulty for granulation and aftertreatment, especially in producing summer, owing to temperature height, high humidity; the very easy humidifying of granulation loop, scab, stop up, cause production not smooth.For overcoming these deficiencies, chemistry expert in various countries' is devoted to explore the production technology and the suitable operating parameters of urea-base compound fertilizer for many years.
The traditional processing technology of urea-base compound fertilizer is that urea and other base fertilizer is broken respectively, joins the granulating of reuniting in the granulating system, though this technology is simple, because prilling temperature is lower, granulation discharging water content is big, thereby strengthened drying load, and the granule strength of product is lower.Chinese patent CN1280969A discloses a kind of method that adopts preparing composite N-P-K fertilizer directly from urea solution; this process using urea production producer concentration is 65.0～99.7%, temperature is 80～140 ℃ urea soln; spray in the tablets press and other base fertilizer reunion granulating; the urea soln that this technology has rationally utilized urea plant to produce; improved prilling temperature; but this technology is more suitable in the producer that urea plant is arranged, and therefore certain limitation is arranged.Also has urea melting technology in addition; be about to solid urea under 110～120 ℃; make～95% urea melting liquid; this urea melting liquid is sprayed in the tablets press and other base fertilizer reunion granulating; the heat energy of this technology utilization urea melting liquid; improved prilling temperature; improved the performance of particle; but owing to the steam energy consumption is increased urea melting; and urea is under higher temperature; facile hydrolysis particularly easily generates the deleterious biuret impurity of crop growth, and the complex fertilizer product quality can not be guaranteed completely.
Summary of the invention
The purpose of this invention is to provide a kind of production method with higher turndown ratio, low returning charge, less energy-consumption, Biuret Content is low, cost is low, quality is high urea-base compound fertilizer.
For achieving the above object, the present invention takes following technical scheme:
A kind of preparation method of urea-base compound fertilizer, its step is as follows:
(1) earlier urea and sulfuric acid, water reaction are generated ureasulfuric acid solution;
(2) gained ureasulfuric acid solution and liquefied ammonia are added the making of base fertilizer that nitrogenous, phosphorus, potassium are housed respectively and carry out aminating reaction in the materials device, and form material with the common granulation of base fertilizer;
(3) gained material drying, cooling, screening; Get the granular urine based compound fertilizer.
The mol ratio of urea and described sulfuric acid, water is 1.6: 1 described in the described step (1): 1-4.5: 1: 1; Be preferably 1.8: 1: 1 or 3.6: 1: 1.
The add-on of ureasulfuric acid solution described in the described step (2) is for adding 10～60% of the total weight in kind of fertilizer.
The total material object of described adding fertilizer comprises base fertilizer, liquefied ammonia of ureasulfuric acid, nitrogenous, phosphorus, potassium etc.
Described ureasulfuric acid solution is through nozzles spray granulation to the material bed of described prilling granulator.
For some kind fertilizer, according to the needs of prescription, be to reduce the solid materials add-on and improve prilling temperature, then described ureasulfuric acid solution also can mix with additional sulfuric acid and/or phosphoric acid after nozzles spray granulation to the material bed of described prilling granulator.
Described liquefied ammonia can be earlier and sulfuric acid or phosphoric acid and washings in neutralizing well or tubular reactor, react, carry, spray into prilling granulator material bed again, carry out granulation with other material.
Described washings is the aqueous solution that contains ammonium sulfate, phosphorus ammonium and other dust.
Described ureasulfuric acid is in described prilling granulator and from spray ammonia axle or spray the liquefied ammonia generation neutralization reaction that the ammonia pipe sprays, and is called aminating reaction.
The time of described aminating reaction is 3～10 minutes.
The temperature of described granulation is 60～90 ℃, is preferably 65～75 ℃.
The time of described granulation is 3～20 minutes.
The base fertilizer of described nitrogenous, phosphorus, potassium is one or more the mixture in monoammonium phosphate, diammonium phosphate, ammonium chloride, ammonium sulfate, general calcium, double superhosphate, fused(calcium magnesium)phosphate, Repone K, vitriolate of tartar, the saltpetre.
Also can add a certain amount of filler in the described prilling granulator; Described filler is one or more the mixture in pulverous wilkinite, kaolin, china clay, potter's clay, phosphogypsum, flyash, talcum powder or the carclazyte; Its add-on is 1%～20% of total weight in kind.
As drying medium, the hot air temperature that enters drying installation generally is controlled at 40～140 ℃ to described drying by warm air.
Temperature of reaction by the described ureasulfuric acid of refrigeration cycle water management is at 60～80 ℃.
The base fertilizer of described nitrogenous, phosphorus, potassium is broken into the pulverulent material less than 1 millimeter before adding prilling granulator.
Principle of the present invention is: urea and sulfuric acid reaction can form ureasulfuric acid, and when reaction system has water to exist, reaction product will be very stable.Show and experimental verification by data, urea, sulfuric acid, water can react the product that generates the different structure transitivity under different mol ratios, mol ratio at urea, sulfuric acid, water is 1.8: 1: 1 and 3.6: 1: 1 o'clock, the ureasulfuric acid product that forms has lower Tc (about 10 ℃), it is 3.6: 1: 1 o'clock particularly in mol ratio, not only its ctystallizing point is minimum, and generates the easier control of reaction of ureasulfuric acid.
The reaction that urea, sulfuric acid, water generate ureasulfuric acid is thermopositive reaction, and control reaction temperature is most important in suitable scope, should adopt effective cooling system, and this reaction heat is in time shifted out, and the invention provides two kinds of cooling temperature control means:
1, in reactive tank, add in cold heat exchanger, with cooling circulating water as heat-eliminating medium.
2, reaction product is fed external heat exchanger, as heat-eliminating medium, the reaction product after the heat exchange is returned reactive tank with cooling circulating water.
3, the temperature of above-mentioned cooling circulating water≤28 ℃.
Temperature of reaction when ureasulfuric acid prepares is controlled at 60～80 ℃, preferably be controlled at 65～75 ℃, so both guaranteed the speed of reaction, guaranteed that again reaction system carries out smoothly under safety, moderate condition, and in this temperature range, the generation of hydrolysis of urea and biuret is very little.
The not only stable performance of ureasulfuric acid product that forms by above-mentioned reaction, when temperature was 60 ℃～80 ℃, its viscosity is lower, and (20～60cps), flowability was fine, and have stronger acidity (pH value is 1.2～1.4), neutralization reaction fast can take place with ammonia (liquefied ammonia, gas ammonia).
During the ureasulfuric acid aminating reaction, as PH during in 2.0 left and right sides, begin to separate out crystal, when reaction reached terminal point, PH was about 5.0.Analyze by the X diffracting spectrum to the ureasulfuric acid aminate, the main thing of ureasulfuric acid aminate is ammonium sulfate and urea mutually, and other has a small amount of unreacted ureasulfuric acid, illustrates with urea bonded sulfuric acid to be converted into ammonium sulfate basically.
Material enters operations such as follow-up screening, fragmentation, cooling, parcel through behind the drying machine, last qualified product weighing and bagging.
Obtain by above-mentioned all process steps that product appearance is mellow and full, granule strength is higher, the urea-base compound fertilizer product of Biuret Content extremely low (≤0.5%).
The existing urea-base compound fertilizer production method of the present invention is compared and is had the following advantages:
1, because the reaction of urea and sulfuric acid, water reaction formation ureasulfuric acid is thermopositive reaction, do not need heat solid urea can form runny ureasulfuric acid liquid, the urea melting method can be saved a large amount of steam consumptions relatively, and this temperature of reaction is controlled at 60～80 ℃, temperature is lower, the hydrolysis of urea is few, and the biuret growing amount that urea condensation generates is extremely low, and the loss of nutrient less, the product mass-energy of product guaranteed completely.
2, the ureasulfuric acid flow of solution that the present invention generated is good, and Tc lower (10～15 ℃) adopts common companion's heat and insulation measure can satisfy the requirement that liquid is carried, and can save the investment of equipment and pipeline greatly.And, can prevent effectively that also pipeline high temperature from mixing the generation that heat causes hydrolysis and biuret.
3, the ureasulfuric acid liquid viscosity is higher, can reach 50cps at 60 ℃, sprays in the tablets press and the easier granulating of other base fertilizer, and product appearance is mellow and full.
4, made full use of the reaction heat that urea, sulfuric acid, water generate ureasulfuric acid solution, and the aminating reaction heat of ureasulfuric acid, energy consumption is reduced; And because the content of water is very low in the ureasulfuric acid solution, make that the particIe system moisture content is lower, also greatly reduce the hot blast load of drying machine; Can realize not having drying or lack the requirement that drying can reach moisture content for some prescription.
5, can solve among the present invention in the granulation process, the problem of powdery ammonium sulfate granulating difficulty is particularly worked as kind and is required the ammonium sulfate add-on more for a long time.
6, among the present invention, utilize the formation reaction heat of ureasulfuric acid and the aminating reaction heat of ureasulfuric acid, prilling temperature is reached about 70 ℃, make the more traditional granulation process of particle intensity want high, make particle intensity higher if add the tubular reactor spray granulating.
7, the easier realization serialization of the present invention is operated automatically, and no matter ureasulfuric acid is prepared or ammoniation-granulation, all has higher turndown ratio, easily control.
8, among the present invention, the aminate of ureasulfuric acid and with other base fertilizer mixing granulating after the critical relative humidity of product pellet can reach more than 60%, even the operation that summer, production also can be unobstructed at high temperature, high humidity, the phenomenon that scabs is not serious, when particularly producing the high nitrogen fertilizer material, effect is more obvious.
Below by embodiment the present invention is further elaborated, but does not mean limiting the scope of the invention.
Embodiment
Embodiment 1
162 kilograms of urea (containing N46%), 79 kilograms of vitriol oils (98%), 8 kg of water are joined the Preparation tank that has agitator respectively simultaneously, in the process that adds, keep a close eye on the Preparation tank variation of temperature, by cooling circulating water temperature of reaction is controlled at 60～80 ℃, through about 40 minutes, reaction finishes, and generates clarifying ureasulfuric acid solution.
With the ureasulfuric acid solution of above-mentioned preparation in mixing tank with 63.7 kilograms the vitriol oil (98%) uniform mixing, after the mixing together through nozzles spray in tablets press.
There is powder ammonium phosphate (to contain N 11%, P in the tablets press
2O
544%) 341 kilograms, Repone K (contains K
2O 60%) 250,64 kilograms of wilkinites are opened spray ammonia axle (or spray ammonia pipe) liquefied ammonia valve, 46 kilograms of liquefied ammonia of spray feed in tablets press simultaneously.
Through granulation in about 5 minutes, it is about 1.5% that about 70 ℃ of prilling temperature, granulation material go out the water content of tablets press mouth, balling ratio 95%.
Material after the granulation is dry in drying machine with the about 110 ℃ hot blast of temperature, and dried material just obtains the compound manure that granularity is 1～4mm through cooling, screening.
Fertilizer product analytical results: N 15.04, P
2O
514.92, K
2O 15.12%, total available nutrient (N+P
2O
5+ K
2O)=45.08%, fertilizer moisture content is 0.8%, and Biuret Content 0.2%, intensity are 35 newton, balling ratio 93%.
Embodiment 2:
383 kilograms of urea (containing N46%), 188 kilograms of vitriol oils (93%), 18.4 kg of water are joined the Preparation tank that has agitator respectively simultaneously, in the process that adds, keep a close eye on the Preparation tank variation of temperature, by cooling circulating water temperature of reaction is controlled at 60～80 ℃, through about 20 minutes, reaction finishes, and generates clarifying ureasulfuric acid solution.
With the ureasulfuric acid solution of above-mentioned preparation through nozzles spray in tablets press.
Meanwhile 29.1 kilograms of liquefied ammonia, 14.8 kilograms of vitriol oils (93%), 210.5 kilograms of phosphoric acid (are contained P
2O
547.5%, water 23.4%) be delivered to tubular reactor through metering, spray in the tablets press after the reaction.
There is Repone K (to contain K in the tablets press
2O 60%) 167 kilograms, open spray ammonia axle (or spray ammonia pipe) liquefied ammonia valve simultaneously, 61.0 kilograms of liquefied ammonia of spray feed in tablets press.
Through granulation in about 5 minutes, it is about 1.4% that about 75 ℃ of prilling temperature, granulation material go out the water content of tablets press mouth, balling ratio 96%.
Material after the granulation is dry in drying machine with the about 110 ℃ hot blast of temperature, and dried material just obtains the compound manure that granularity is 1～4mm through cooling, screening.
Fertilizer product analytical results: N 25.12, P
2O
510.04, K
2O 9.89%, total available nutrient (N+P
2O
5+ K2O)=45.05%, fertilizer moisture content is 0.7%, Biuret Content 0.2%, intensity are 29 newton, balling ratio 93%.
Embodiment 3
383 kilograms of urea (containing N46%), 188 kilograms of vitriol oils (93%), 18.4 kg of water are joined the Preparation tank that has agitator respectively simultaneously, in the process that adds, keep a close eye on the Preparation tank variation of temperature, by cooling circulating water temperature of reaction is controlled at 60～80 ℃, through about 20 minutes, reaction finishes, and generates clarifying ureasulfuric acid solution.
With the ureasulfuric acid solution of above-mentioned preparation through nozzles spray in tablets press.
Meanwhile 29.1 kilograms of liquefied ammonia, 210.5 kilograms of phosphoric acid (are contained P
2O
547.5%, water 23.4%) be delivered to neutralizing well through metering, spray in the tablets press after the reaction.
There is Repone K (to contain K in the tablets press
2O 60%) 167 kilograms, open spray ammonia axle (or spray ammonia pipe) liquefied ammonia valve simultaneously, 61.0 kilograms of liquefied ammonia of spray feed in tablets press.
Through granulation in about 5 minutes, it is about 1.4% that about 75 ℃ of prilling temperature, granulation material go out the water content of tablets press mouth, balling ratio 96%.
Material after the granulation is dry in drying machine with the about 110 ℃ hot blast of temperature, and dried material just obtains the compound manure that granularity is 1～4mm through cooling, screening.
Fertilizer product analytical results: N 25.12, P
2O
510.04, K
2O 9.89%, total available nutrient (N+P
2O
5+ K
2O)=45.05%, fertilizer moisture content is 0.7%, and Biuret Content 0.2%, intensity are 29 newton, balling ratio 93%.
Embodiment 4
277 kilograms of urea (containing N46%), 210 kilograms of vitriol oils (98%), 33.6 kg of water are joined the Preparation tank that has agitator respectively simultaneously, in the process that adds, keep a close eye on the Preparation tank variation of temperature, by cooling circulating water temperature of reaction is controlled at 60～80 ℃, through about 40 minutes, reaction finishes, and generates clarifying ureasulfuric acid solution.
With the ureasulfuric acid solution of above-mentioned preparation in mixing tank with 56 kilograms phosphoric acid (P
2O
5Content 50%) uniform mixing, after the mixing together through nozzles spray in tablets press.
There is powder ammonium phosphate (to contain N 11%, P in the tablets press
2O
544%) 50 kilograms, Repone K (contains K
2O 60%) 168,180 kilograms of kaolin are opened spray ammonia axle (or spray ammonia pipe) liquefied ammonia valve, 82 kilograms of liquefied ammonia of spray feed in tablets press simultaneously.
Through granulation in about 5 minutes, it is about 1.5% that about 70 ℃ of prilling temperature, granulation material go out the water content of tablets press mouth, balling ratio 95%.
Material after the granulation is dry in drying machine with the about 110 ℃ hot blast of temperature, and dried material just obtains the compound manure that granularity is 1～4mm through cooling, screening.
Fertilizer product analytical results: N 20.14, P
2O
55.02, K
2O 10.13%, total available nutrient (N+P
2O
5+ K
2O)=45.08%, fertilizer moisture content is 0.8%, and Biuret Content 0.15%, intensity are 30 newton, balling ratio 93%.
In the foregoing description, each analysis project of compound manure and analytical procedure are according to the fertile quality standard GB15063-2001 of national compound; Atomic absorption method is adopted in the detection of biuret in the composite fertilizer.
Claims (17)
1, a kind of preparation method of urea-base compound fertilizer, its step is as follows:
(1) earlier urea and sulfuric acid, water reaction are generated ureasulfuric acid solution;
(2) gained ureasulfuric acid solution and liquefied ammonia are added the making of base fertilizer that nitrogenous, phosphorus, potassium are housed respectively and carry out aminating reaction in the materials device, and form material with the common granulation of base fertilizer;
(3) gained material drying, cooling, screening; Get the granular urine based compound fertilizer.
2, the preparation method of urea-base compound fertilizer according to claim 1 is characterized in that: ureasulfuric acid solution described in the described step (2) mixes with sulfuric acid and/or phosphoric acid earlier, adds described prilling granulator again.
3, the preparation method of urea-base compound fertilizer according to claim 1, it is characterized in that: liquefied ammonia described in the described step (2) reacts in neutralizing well or tubular reactor with sulfuric acid or phosphoric acid and the washings that contains ammonium sulfate, phosphorus ammonium and other dust earlier, adds described prilling granulator again.
4, as the preparation method of urea-base compound fertilizer as described in each in the claim 1～3, it is characterized in that: the mol ratio of urea and sulfuric acid, water is 1.6: 1: 1～4.5: 1: 1 described in the described step (1).
5, as the preparation method of urea-base compound fertilizer as described in the claim 4, it is characterized in that: the add-on of ureasulfuric acid solution described in the described step (2) is for adding 10～60% of the total weight in kind of fertilizer.
6, as the preparation method of urea-base compound fertilizer as described in the claim 5, it is characterized in that: the total material object of described adding fertilizer comprises ureasulfuric acid, nitrogenous, phosphorus, base fertilizer, liquefied ammonia and/or sulfuric acid, the phosphoric acid of potassium and the washings that contains ammonium sulfate, phosphorus ammonium and other dust.
7, as the preparation method of urea-base compound fertilizer as described in the claim 6, it is characterized in that: the temperature of described granulation is 60～90 ℃.
8, as the preparation method of urea-base compound fertilizer as described in the claim 6, it is characterized in that: the temperature of described granulation is 65～75 ℃.
9, as the preparation method of urea-base compound fertilizer as described in the claim 8, it is characterized in that: the time of described granulation is 3～20 minutes.
10, as the preparation method of urea-based compound fertilizer as described in each in the claim 1～3, it is characterized in that: the base fertilizer of nitrogenous, the phosphorus described in the described step (2), potassium is one or more the mixture in monoammonium phosphate, diammonium phosphate, ammonium chloride, ammonium sulfate, general calcium, double superhosphate, fused(calcium magnesium)phosphate, Repone K, vitriolate of tartar or the saltpetre.
11, as the preparation method of urea-base compound fertilizer as described in each in the claim 1～3, it is characterized in that: described hot blast temperature when dry is 60～140 ℃.
12, as the preparation method of urea-base compound fertilizer as described in each in the claim 1～3, it is characterized in that: the mol ratio of urea, sulfuric acid, water is 1.8: 1: 1 or 3.6: 1: 1 described in the described step (1).
13, as the preparation method of urea-base compound fertilizer as described in each in the claim 1～3, it is characterized in that: the temperature of reaction by the described ureasulfuric acid of the described step of refrigeration cycle water management (1) is at 60～80 ℃.
14, as the preparation method of urea-base compound fertilizer as described in each in the claim 1～3, it is characterized in that: the temperature of reaction by the described ureasulfuric acid of the described step of refrigeration cycle water management (1) is at 65～75 ℃.
15, as the preparation method of urea-base compound fertilizer as described in each in the claim 1～3, it is characterized in that: add filler in the described prilling granulator.
16, as the preparation method of urea-base compound fertilizer as described in the claim 15, it is characterized in that: described filler is one or more the mixture in pulverous wilkinite, kaolin, china clay, potter's clay, phosphogypsum, flyash, talcum powder or the carclazyte.
17, as the preparation method of urea-base compound fertilizer as described in the claim 16, it is characterized in that: the amount of described filler is for adding 1%～20% of the total weight in kind of fertilizer.
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