CN102070358B - Method for preparing round and granular potassic fertilizer by utilizing post precipitation salt of phosphoric acid - Google Patents
Method for preparing round and granular potassic fertilizer by utilizing post precipitation salt of phosphoric acid Download PDFInfo
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- CN102070358B CN102070358B CN 201010548138 CN201010548138A CN102070358B CN 102070358 B CN102070358 B CN 102070358B CN 201010548138 CN201010548138 CN 201010548138 CN 201010548138 A CN201010548138 A CN 201010548138A CN 102070358 B CN102070358 B CN 102070358B
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- phosphoric acid
- postprecipitation
- slip
- sylvite
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Abstract
The invention discloses a method for preparing round and granular potassic fertilizer, comprising the following steps of: (1) putting post precipitation salt slurry of wet-process phosphoric acid into a container, regulating the content of solid phase of the post precipitation salt to be 40-60% by adding phosphoric acid and/or water, simultaneously controlling the mass concentration of P2O5 in the post precipitation salt slurry to be 30%-40% and obtaining post precipitation salt slurry A of the phosphoric acid; (2) spraying the post precipitation salt slurry A of the phosphoric acid accounting for 20.0-30.0% of the total mass of raw materials on a return bed in a rotary drum granulating device, simultaneously introducing ammonia accounting for 1.0-2.0% of the total mass of raw materials, neutralizing the post precipitation salt slurry A of the phosphoric acid; then putting potassium salt accounting for 68.0-79.0% of the raw materials into a return circulating system in the rotary drum granulating device, and then carrying out granulation; and (3) drying, screening and cooling the granulates to obtain a qualified product. In the method disclosed by the invention, the technology is reasonable, the production cost is low, large-scale industrial production is easy, and better economic and social benefits can be generated.
Description
Technical field
The present invention relates to a kind of method of utilizing phosphoric acid postprecipitation salt to prepare circular granular potash fertilizer.
Background technology
The developmental stage from the straight fertilizer to the compound manure has been passed through in the production of chemical fertilizer and use, has begun to enter into the fertilising stage of surveying the soil prescription.Fertilization compositions based on earth measurement is the fertility situation according to nutritional needs and the soil of plant, uses the fertilizer of proper ratio nutrient.Straight fertilizer, the compound manure of industrialized mass because of the kind limited amount of product, are difficult to satisfy preferably the needs of fertilization compositions based on earth measurement at present.A kind of production method that is referred to as bulk blended fertilizer is arranged, namely according to the nutrient ratio requirement, take the various solid base fertilizers such as the basically identical nitrogen of obvious chemical reaction, granularity and circularity, phosphorus, potassium that do not occur as raw material, the method by blending is mixed with the uniform fertilizer of Nutrient distribution.This fertilizer course of processing is simple, and plant investment expense and processing charges are lower, is a kind of fertilizer variety that is very suitable for fertilization compositions based on earth measurement.This fertilizer when production, accumulating, use, extremely emphasize various base fertilizers particle size, severe and circularity basically identical, make and occur that caking is pulverized and the phenomenon of low moisture absorption point after the unlikely generation blending.
Production is best suited for the bulk blended fertilizer kind of fertilization compositions based on earth measurement demand, the agglomeration technique of the circular granular simple substance base fertilizer of present needed nitrogenous fertilizer, phosphate fertilizer is very ripe, but the base fertilizer of potassium, what generally adopt at present both at home and abroad is the extruder grain technology, the granular potash fertilizer product that this technology is produced, the irregular particle of a kind of sheet (and the throughput of single series production equipment is lower, is generally ten thousand ton/years of 1-5).
The employed potassium base fertilizer of bulk blended fertilizer in the existing market, because what generally use is the irregular particle of sheet, easily segregation layering in storage and transport process makes nutrient difference large (the sale radius of U.S.'s restriction bulk blended fertilizer product should in 60 kilometers).For the base fertilizer that overcomes potassium in the bulk blended fertilizer production is the defective of sheet irregular particle; had in recent years and utilize rotary drum granulator by the method for steam with powdery sylvite and clay agglomeration granulation; this method generally needs relatively large steam and clay; production cost is higher; the content of effective constituent potassium is lower, is not suitable for scale operation.Also have by adding high polymer binder to be configured to the aqueous solution sylvite of powdery is carried out agglomeration granulation, because binding agent is expensive, granulation need use steam equally, and sylvite needs the operations such as further pulverizing, and production cost is higher, is difficult to realize industrialization.
Phosphoric acid by wet process is for the production of the history in existing more than 100 year of fertilizer, and production technique is very mature and stable.But in the concentrated and storage process of phosphoric acid extraction, along with the variation of temperature and time, have a large amount of solid phase postprecipitation salt and produce (mainly being the composite salt of iron aluminium), the viscosity of this postprecipitation salt is very large.At present, the enterprise of Wet-process Phosphoric Acid Production fertilizer, treatment process to the postprecipitation salt of phosphoric acid, after normally adopting natural subsidence to separate, the one, send extraction or filter progress back to and again carry out washing and filtering, this method can reduce the ability of extraction and filtration unit to a certain extent, and affects the detersive efficiency of filter progress; The 2nd, be configured in proportion certain P with the phosphoric acid of clarifying
2O
5Concentration, be used for to give birth to ammonium phosphate fertilizers (for example MAP), this method can make the P in the product
2O
5% descends to some extent; The 3rd, the periodic cleaning phosphoric acid storage tank out is used for the phosphoric acid postprecipitation salt of solid phase to process general calcareous fertilisers material etc. by the labor cleaning, and this method need to expend a large amount of manpower and materials.
Therefore, the production method of circular granular potassium base fertilizer of (take sylvite and phosphoric acid by wet process postprecipitation salt as raw material) just becomes the technical barrier that this technical field is needed solution badly to provide that a kind of technique is reasonable and production cost is low.
Summary of the invention
The production method that the purpose of this invention is to provide the circular granular potash fertilizer that a kind of technique is reasonable and production cost is low.
The method for preparing circular granular potash fertilizer provided by the present invention comprises the steps:
(1) phosphoric acid by wet process postprecipitation salt slip is placed container, by adding phosphoric acid and/or water, the solid phase matter content of regulating and control its postprecipitation salt is 40-60% (to keep good flowability), controls simultaneously P in the described postprecipitation salt slip
2O
5Mass concentration be 30%-40%, obtain phosphoric acid postprecipitation salt slip A;
(2) in the drum granulating device, drop in sylvite and the ammonification and after phosphoric acid postprecipitation salt slip dry material as bed material, make the circular flow of bed material reach 3-5 times that drops into the raw material total mass when device moves, the starting granulation returning charge recycle system, and system is preheated to the bed material temperature reaches 60-70 ℃;
In the described ammonification and after phosphoric acid postprecipitation salt slip dry material by phosphoric acid postprecipitation salt slip A and ammonia according to mass ratio (20-30): (1-2) reaction obtains, in the described bed material in sylvite and the ammonification with after phosphoric acid postprecipitation salt slip dry material mass ratio be (68-79): (21-32);
Described raw material is that material forms by following mass percent: the described phosphoric acid postprecipitation of 20.0-30.0% salt slip A, the ammonia of 1.0-2.0% and the sylvite of 68.0-79.0%;
(3) with the phosphoric acid postprecipitation salt slip A in the described raw material, send into the drum granulating device that bed material is housed in the step (2) by shurry pump, on shower nozzle is sprayed at returning charge bed in the drum granulating device, in described returning charge bed, pass into simultaneously the ammonia in the described raw material, described phosphoric acid postprecipitation salt slip A is neutralized;
Or the phosphoric acid postprecipitation salt slip A in the described raw material sent into tubular reactor, in described tubular reactor, add simultaneously the ammonia in the described raw material, described phosphoric acid postprecipitation salt slip A is neutralized, and the slip after will neutralizing again is sprayed on the returning charge bed of drum granulating device;
(4) the returning charge recycle system in the drum granulating device drops into sylvite in the described raw material again, forms the semi-product material of water content 3-5%;
(5) semi-product material of step (4) gained is carried out drying, obtain circular granular potash fertilizer.
The circular granular potash fertilizer that aforesaid method prepares obtains the circular granular potash fertilizer that particle diameter is 2-4.75mm through screening.In the above-mentioned steps, the quality of the quality of described raw material total mass, phosphoric acid postprecipitation salt slip A, the quality of ammonia and sylvite is all in butt.
Wherein, the sylvite described in step (2) and (4) is Repone K or vitriolate of tartar; The purity of described sylvite in the potassium oxide mass content greater than 〉=50%.
Backing material formula is described in the step (2): the Repone K of 680-790kg/t (butt, lower same) or vitriolate of tartar; In the ammonification and after phosphoric acid postprecipitation salt slip dry material 210-320kg/t.The proportioning of required each raw material is consistent when making backing material formula with preparing product, is conducive to produce fast qualified product.
Step 4) water content in the semi-product material can be controlled by water content, the flow of returning charge and the thermal load of drying machine of controlling the postprecipitation salt A that adds.
Adopting temperature from roasting kiln in the step (5) is that 350-450 ℃ hot gas carries out drying to described semi-product material, dry after the temperature of product be 70-90 ℃.
The main component of phosphoric acid postprecipitation salt is in the used phosphoric acid postprecipitation salt slip of the present invention:
(F
e, Al)
3KH
14(PO)
84H
2O; (N
a, K)
2SiF
6C
aSO
40.5H
2O; AlH
3(PO
4)
22H
2O; C
aSO
42H
2O; Na
XMg
XAl
2-X, (F, OH)
6H
2O; (Mg, Fe, M
n) SiF
6H
2O etc.
The circular granular potassium base fertilizer that the present invention is prepared had both contained higher K
2The main nutrient of O also contains a certain amount of P
2O
5And N, also contain the middle trace plant nutrition such as a certain amount of Ca, Mg, Si and divide element; This product both can be used separately according to plants and soil fertility situation, more can use with blending such as particle nitrogen fertilizer, granulated phosphate fertilizer or composite fertilizers, can satisfy to greatest extent fertilization compositions based on earth measurement to the market requirement of fertilizer variety; The phosphoric acid postprecipitation salt that the present invention adopts phosphorus compound fertilizer enterprise liquid extraction phosphoric acid to produce in concentrated and storage process is produced the circular granular potassium base fertilizer, can solve present phosphorus compound fertilizer enterprise and send phosphoric acid by wet process postprecipitation salt back to the extraction filtration unit, the production capacity of impact extraction filtration unit and the problem of washing rate, or with phosphoric acid postprecipitation salt for the production of ammonium phosphate fertilizers, can reduce the problem of product nutrient.Because the tough physics-chem characteristic of postprecipitation salt slip of phosphoric acid by wet process makes it bring into play the effect of tackiness agent in sylvite (particularly Repone K mostly is the grittiness material) granulation, thereby has reduced production cost.And the method technique rationally is easy to realize large-scale industrial production, can produce preferably economic benefit and social benefit.
Embodiment
Below by specific embodiment method of the present invention is described, but the present invention is not limited thereto.
Experimental technique described in the following embodiment if no special instructions, is ordinary method; Described reagent and material if no special instructions, all can obtain from commercial channels.Phosphoric acid postprecipitation salt used among the following embodiment is the by product that produces in the production process of phosphoric acid." % " described in the following embodiment is " quality percentage composition ".
Embodiment 1, " 2-13-40 " contain the production that potassium is master's chloro circular granular potassium base fertilizer
Press the ratio of phosphoric acid postprecipitation salt slip (butt, lower with)/synthetic ammonia/sylvite=30: 2: 68, composition of raw materials is: phosphoric acid postprecipitation salt solids in pulp amount is 60%, contain P
2O
5%30.0 (wherein contains H
3PO
4Shared P
2O
5%18.0; H
2O%30): 428.57kg/t; Synthetic ammonia (HN
3%99.5; H
2O%0.5) 18.56kg/t; Repone K: 688.42kg/t (60%K
2O, H
2O%1.0).
Production stage is as follows:
(1) mass ratio by 68: 32 drops into Repone K (60%K in rotary drum granulator
2O) and in ammonification and after phosphoric acid postprecipitation salt slip dry material as bed material, the circular flow 200-250t/h of bed material, reach the 4-5 of the raw material total mass that will drop into the drum granulating device doubly, the starting granulation returning charge recycle system, and system is preheated to the bed material temperature reaches 60-70 ℃;
(2) starting phosphoric acid postprecipitation salt shurry pump, with phosphoric acid postprecipitation salt slip, send into the drum granulating device by the flow of 21.43t/h, by shower nozzle slip is sprayed on the returning charge bed, the synthetic ammonia that the ammonia sparger of while in the returning charge bed passes into 0.93t/h neutralizes phosphoric acid postprecipitation salt slip (or with phosphoric acid postprecipitation salt slip, flow by 21.43t/h is sent into tubular reactor, synthetic ammonia to tubular reactor adding 0.93t/h neutralizes phosphoric acid postprecipitation salt slip simultaneously, be sprayed on the returning charge bed after making reaction slurry), meanwhile press composition of raw materials and press the flow input Repone K of 34.42t/h in the returning charge recycle system of drum granulating device, go out the semi-product material that the interruption-forming water content is 3-4% at tablets press;
(3) semi-product material drying (drying machine is 400-450 ℃ from the hot air temperature of roasting kiln, and the temperature of dry rear product is 70-90 ℃, and the residence time of material in drying machine is 50 minutes); Screening (aperture of levels screen cloth be respectively 4.75 and 2.00mm); Cooling (be 40-50 ℃ after the product cooling, the residence time of product in cooler is 20 minutes), namely obtaining particle diameter is the product that potassium is master's circular granular base fertilizer that contains of 2-4.75mm.
The product specification of producing by this composition of raw materials is (2-13-40): N%=1.52; P
2O
5%=12.86; K
2O%=41.30; H
2O%=2.0; Granularity (2-4.75mm%) 〉=90; Granule strength 〉=20N.
Embodiment 2, " 1-10-40 " contain the production that potassium is master's sulfenyl circular granular potassium base fertilizer
Press phosphoric acid postprecipitation salt slip (butt, lower with): synthetic ammonia: the ratio of sylvite=20: 1: 79, composition of raw materials is: phosphoric acid postprecipitation salt solids in pulp amount is 40%, contain P
2O
5%40.0 (wherein contains H
3PO
4Shared P
2O
5%20.0; H
2O%25): 266.67kg/t; Synthetic ammonia (HN
3%99.5; H
2O%0.5) 12.83kg/t; Vitriolate of tartar: 795.18kg/t (50%K
2O, H
2O%1.0).
Production stage is as follows:
(1) mass ratio by 79: 21 drops into vitriolate of tartar (50%K in rotary drum granulator
2O) and in the via nitride and after the bed material of phosphoric acid postprecipitation salt slip dry material, the circular flow 200-250t/h of bed material, reach the 4-5 of the raw material total mass that will drop into the drum granulating device doubly, the starting granulation returning charge recycle system, and system is preheated to the bed material temperature reaches 60-70 ℃;
(2), starting phosphoric acid postprecipitation salt shurry pump, with phosphoric acid postprecipitation salt slip, send into the drum granulating device by the flow of 13.334t/h, by shower nozzle slip is sprayed on the returning charge bed, the synthetic ammonia that the ammonia sparger of while in the returning charge bed passes into 0.642t/h neutralizes phosphoric acid postprecipitation salt slip (or with phosphoric acid postprecipitation salt slip, flow by 26.667t/h is sent into tubular reactor, synthetic ammonia to tubular reactor adding 0.642t/h neutralizes phosphoric acid postprecipitation salt slip simultaneously, be sprayed on the returning charge bed after making reaction slurry), meanwhile press composition of raw materials and press the flow input vitriolate of tartar of 39.76t/h in the returning charge recycle system of drum granulating device, go out the semi-product material that the interruption-forming water content is 3-4% at tablets press;
(3) semi-product material drying (drying machine is 400-450 ℃ from the hot air temperature of roasting kiln, and the temperature of dry rear product is 70-90 ℃, and the residence time of material in drying machine is 50 minutes); Screening (aperture of levels screen cloth be respectively 4.75 and 2.00mm); Cooling (be 40-50 ℃ after the product cooling, the residence time of product in cooler is 20 minutes), namely obtaining particle diameter is the product that potassium is master's circular granular base fertilizer that contains of 2-4.75mm.
The product specification of producing by this composition of raw materials is (1-10-40): N%=1.05; P
2O
5%=10.67; K
2O%=39.76; H
2O%=1.50; Granularity (2-4.75mm%) 〉=90; Granule strength 〉=25N.
The outstanding advantages of the circular granular potassium base fertilizer of above-described embodiment preparation is:
1. contain higher K in the product
2O (〉=40%) contains a certain amount of P simultaneously
2O
5Outside the inorganic nutrients of N, according to the fertility situation of soil, can use separately, be that a kind of potassium that contains efficiently is main base fertilizer.
2. product compares with the platy shaped particle potash fertilizer that generally is used as at present bulk blended fertilizer both at home and abroad as the base fertilizer of Bulk Blending Fertilizer, and product is circular granular, can overcome bulk blended fertilizer and easily produce the defective that the segregation layering affects quality product.
3. the production technology of this product, compare (the single series unit scale is ten thousand ton/years of 1-5) with the basic fertilizer that generally is at present employing extruder grain production sheet potassium both at home and abroad, production equipment can be realized maximizing (〉=30 ten thousand ton/years), can produce preferably scale and benefit.
Claims (4)
1. a method for preparing circular granular potash fertilizer comprises the steps:
(1) phosphoric acid by wet process postprecipitation salt slip is placed container, by adding phosphoric acid and/or water, the solid phase matter content of regulating and control its postprecipitation salt is 40-60%, controls simultaneously P in the described postprecipitation salt slip
2O
5Mass concentration be 30%-40%, obtain phosphoric acid postprecipitation salt slip A;
(2) in the drum granulating device, drop in sylvite and the ammonification and after phosphoric acid postprecipitation salt slip dry material as bed material, make the circular flow of bed material reach 3-5 times that drops into the raw material total mass when device moves, the starting granulation returning charge recycle system, and system is preheated to the bed material temperature reaches 60-70 ℃;
In the described ammonification and after phosphoric acid postprecipitation salt slip dry material by phosphoric acid postprecipitation salt slip A and ammonia according to mass ratio (20-30): (1-2) reaction obtains, in the described bed material in sylvite and the ammonification with after phosphoric acid postprecipitation salt slip dry material mass ratio be (68-79): (21-32);
Described raw material is comprised of the material of following mass percent: the described phosphoric acid postprecipitation of 20.0-30.0% salt slip A, the ammonia of 1.0-2.0% and the sylvite of 68.0-79.0%;
(3) with the phosphoric acid postprecipitation salt slip A in the described raw material, send into the drum granulating device that bed material is housed in the step (2) by shurry pump, on shower nozzle is sprayed at returning charge bed in the drum granulating device, in described returning charge bed, pass into simultaneously the ammonia in the described raw material, described phosphoric acid postprecipitation salt slip A is neutralized;
Or the phosphoric acid postprecipitation salt slip A in the described raw material sent into tubular reactor, in described tubular reactor, add simultaneously the ammonia in the described raw material, described phosphoric acid postprecipitation salt slip A is neutralized, and the slip after will neutralizing again is sprayed on the returning charge bed of drum granulating device;
(4) the returning charge recycle system in the drum granulating device drops into sylvite in the described raw material again, forms the semi-product material of water content 3-5%;
(5) semi-product material of step (4) gained is carried out drying, obtain circular granular potash fertilizer;
In the above-mentioned steps, the quality of the quality of described raw material total mass, phosphoric acid postprecipitation salt slip A, the quality of ammonia and sylvite is all in butt.
2. method according to claim 1, it is characterized in that: sylvite is Repone K or vitriolate of tartar described in step (2) and (4); The purity of described sylvite in the potassium oxide mass content greater than 〉=50%.
3. method according to claim 1 is characterized in that: adopting temperature from roasting kiln in the step (5) is that 350-450 ℃ hot gas carries out drying to described semi-product material, dry after the temperature of product be 70-90 ℃.
4. method according to claim 1, it is characterized in that: the particle diameter of described circular granular potash fertilizer is 2-4.75mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010548138 CN102070358B (en) | 2010-11-17 | 2010-11-17 | Method for preparing round and granular potassic fertilizer by utilizing post precipitation salt of phosphoric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010548138 CN102070358B (en) | 2010-11-17 | 2010-11-17 | Method for preparing round and granular potassic fertilizer by utilizing post precipitation salt of phosphoric acid |
Publications (2)
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| CN102070358B true CN102070358B (en) | 2013-05-01 |
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| CN104609919B (en) * | 2014-07-28 | 2017-09-29 | 郑秀兴 | A kind of method of low cost manufacture a great number of elements water-soluble fertilizer |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562896A (en) * | 2004-03-25 | 2005-01-12 | 华南理工大学 | Long acting potasium fertilizer of mineral and preparation method |
| CN101367682A (en) * | 2008-09-28 | 2009-02-18 | 中国-阿拉伯化肥有限公司 | Method for preparing complex fertilizer with mutual solution slip tubular reactor |
| CN101423433A (en) * | 2008-11-27 | 2009-05-06 | 中国-阿拉伯化肥有限公司 | Method for preparing circular granule nitrogen and potassium fertilizer |
| CN101503322A (en) * | 2009-03-10 | 2009-08-12 | 施可丰化工股份有限公司 | Slow release type azophoska compound fertilizer and production method thereof |
| CN101792334A (en) * | 2010-02-10 | 2010-08-04 | 吉林市博达钾肥有限公司 | Spherical potassium chloride particle and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001031488A (en) * | 1999-05-14 | 2001-02-06 | Mitsubishi Chemicals Corp | Production of fertilizer and solid fertilizer |
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2010
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562896A (en) * | 2004-03-25 | 2005-01-12 | 华南理工大学 | Long acting potasium fertilizer of mineral and preparation method |
| CN101367682A (en) * | 2008-09-28 | 2009-02-18 | 中国-阿拉伯化肥有限公司 | Method for preparing complex fertilizer with mutual solution slip tubular reactor |
| CN101423433A (en) * | 2008-11-27 | 2009-05-06 | 中国-阿拉伯化肥有限公司 | Method for preparing circular granule nitrogen and potassium fertilizer |
| CN101503322A (en) * | 2009-03-10 | 2009-08-12 | 施可丰化工股份有限公司 | Slow release type azophoska compound fertilizer and production method thereof |
| CN101792334A (en) * | 2010-02-10 | 2010-08-04 | 吉林市博达钾肥有限公司 | Spherical potassium chloride particle and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| JP特开2001-31488A 2001.02.06 |
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Address after: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee after: China Blue Chemical Ltd. Patentee after: China Offshore Oil Group Co., Ltd. Co-patentee after: Sino-Arab Chemical Fertilizer Co., Ltd. Address before: 100010 Beijing, Chaoyangmen, North Street, No. 25, No. Co-patentee before: China Blue Chemical Ltd. Patentee before: China National Offshore Oil Corporation Co-patentee before: Sino-Arab Chemical Fertilizer Co., Ltd. |
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