CN101200392B - Method for manufacturing powdered granulated potassium ammonium sulfate compound fertilizer - Google Patents
Method for manufacturing powdered granulated potassium ammonium sulfate compound fertilizer Download PDFInfo
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- CN101200392B CN101200392B CN2006101472630A CN200610147263A CN101200392B CN 101200392 B CN101200392 B CN 101200392B CN 2006101472630 A CN2006101472630 A CN 2006101472630A CN 200610147263 A CN200610147263 A CN 200610147263A CN 101200392 B CN101200392 B CN 101200392B
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Abstract
The invention relates to a manufacturing method for granular ammonium-potassium sulfate, which is characterized in that: the potasium bisulfate solution comprising excessive vitriol and a spot of unreacted potassium chloride which is obtained from the low-temperature conversion of vitrol and potassium chloride is mixed with a certain amount of water; the mixed ground paste is implemented on a neutralization reaction with the gaseous ammonia in a tubular reactor; the neutralization ground paste is sprayed into a spray dryer; the moisture in the ground paste is vaporized by the chemical reaction of the neutralization reaction, thereby the granular ammonium-potassium sulfate can be produced directly. The invention has the advantages that the process is simple; the charge of invention and operation is lower; the source of non-potassium chloride material can be broaden, and the secondary processing costs for compound fertilizer can be reduced.
Description
Technical field
The present invention relates to a kind of manufacture method of agrochemical, specifically, relate to a kind of manufacture method that contains the chemical fertilizer of elements such as nitrogen, sulphur, potassium, i.e. the manufacture method of ammonium-potassium sulfate compound manure, this is a kind of method with mist projection granulating manufactured powdered granulated potassium ammonium sulfate.
Background technology
Powder shape fertilizer is an important kind in the chemical fertilizer.It can use separately, also can be used as the basic material of granular compound fertilizer material.The good powder shape fertilizer of quality is subjected to the welcome of agricultural sector and granular compound fertilizer secondary processing enterprise deeply.
Chinese patent (number of patent application 93111207.9) " production method of potassium sulphate type ternary composite fertilizer " has been introduced Repone K and vitriol oil conversion reaction, produce sal enixum, potassium hydrogen sulfate solution mixes with phosphoric acid then, neutralize with ammonia at neutralizing well, spray granulating is made the method for potassium sulphate type ternary composite fertilizer material.
The TVA of the U.S., Spain Cros etc. are raw material with the concentrated phosphoric acid, use tubular reactor and replace traditional slot type to stir ammoniation reactor, and producing ammonium phosphate and ammonium phosphate is compound manure, have obtained multinomial patent (US 3,130,033, US 3,420,624).At present, the tubular reactor produced technology is by many ammonium phosphate and ammonium phosphate are that compound manure manufacturing enterprise adopts in the world.
Britain Fisons company in 1964 has developed slot type pressurization ammonia neutralization and spraying drying is produced powdery monoammonium phosphate production technology (patent No. US 3,415,638).The Swift agricultural of the U.S. has developed the nozzle ammoniation reactor with chemical company and spraying drying is produced powdery monoammonium phosphate production technique (patent No. US 3,419,378).The appearance of above-mentioned Technology has produced bigger pushing effect to the development of chemical fertilizer production technology.
In recent ten years; China's chemical fertilizer industrial development is comparatively rapid; Shanghai Chemical Research Inst reaches in country " six or five " and has carried out powdery monoammonium phosphate manufacturing technology and pipeline reactor system phosphorus ammonium and nitrogen, phosphorus, K composite fertilizer Study on Production Technology in " the Seventh Five-Year Plan " key scientific and technological projects; finished interim test; and promote above-mentioned technology at home, obtained bigger achievement.
Summary of the invention
The present invention is intended to draw the manufacture method and the corresponding technological process of production that a kind of powdered granulated potassium ammonium sulfate is provided on above-mentioned composite chemical fertilizer manufacturing technology and the empirical basis.It is a basic material with the potassium hydrogen sulfate solution that contains excess sulfuric acid and a small amount of unreacted Repone K of sulfuric acid and Repone K low temperature conversion gained, through and after a certain amount of water mixes, in tubular reactor, carry out neutralization reaction with gaseous ammonia.And utilize the chemical reaction heat of raw material, and evaporate moisture, spray-dried again, obtain the powdered granulated potassium ammonium sulfate product.This method technology of directly making the powdered granulated potassium ammonium sulfate product is simple, and investment and process cost are low, can widen no chlorine sylvite raw material sources, the secondary processing expense of reduction composite fertilizer.
The present invention is achieved in that it mainly is a neutralization reaction of utilizing sal enixum and ammonia, it is characterized in that described manufacture method comprises the steps:
(1) being mixed and made into density with the potassium hydrogen sulfate solution that contains excess sulfuric acid and a small amount of unreacted Repone K of sulfuric acid and Repone K low temperature conversion gained and a certain amount of water is 1.58～1.62g/cm
3, temperature is 90～110 ℃ mixed slurry;
(2) mixed slurry carries out neutralization reaction with gaseous ammonia in tubular reactor, 140～160 ℃ of temperature of reaction, and pressure is 0.2～0.4MPa, the pH value of reaction back slip is 4～5;
(3) in the tubular reactor in and slip spray the drying tower from the spraying drying column overhead, in and slip in moisture content be depressurized flash distillation, the fine silt of spraying in the landing process with the freezing air contact heat-exchanging and the cooling drying that rise, at the bottom of tower, obtain the ammonium-potassium sulfate compound manure.
Described Repone K low temperature conversion technology is to adopt the sulfuric acid of excessive 10-20% and Repone K to react down at 120～130 ℃, and reactant is sal enixum, sulfuric acid and a small amount of unreacted Repone K mixed slurry and hydrogen chloride gas.Hydrogen chloride gas adopts falling-film absorber to be absorbed into the hydrochloric acid of concentration about 30% by water, and other uses it for anything else.Be used for making mixed slurry reaction below can taking place of powdered granulated potassium ammonium sulfate compound fertilizer with gaseous ammonia neutral process:
H
2SO
4+NH
3＝(NH
4)
2SO
4
KHSO
4+NH
3＝K
2SO
4+(NH
4)
2SO
4
Above-mentioned reaction process is very quick, and especially the aminating reaction of sulfuric acid and ammonia belongs to reaction at full speed, can produce a large amount of heats.Adding an amount of water in mixed slurry both can increase the flowability of slip, can prevent that also the fast rapid-curing cutback of material in the N-process is solid, stopped up tubular reactor.The add-on of water is adjusted into 1.58～1.62g/cm with the density slip
3Be advisable, temperature also will be controlled at 90～110 ℃.In view of the above, joining the ratio of the water in the potassium hydrogen sulfate solution, in mass, is 0.3～0.7: 1.The add-on of gaseous ammonia need be controlled by ammonia neutral degree by potassium hydrogen sulfate solution in the tubular reactor, and the slip pH value with terminal point in this moment is 4～5.
When implementing the inventive method, can adopt following technical process: liquefied ammonia changes into gaseous ammonia by vaporizer, sends into the gaseous ammonia buffer tank and delivers to tubular reactor after metering; In addition, the potassium hydrogen sulfate solution of sulfuric acid and Repone K low temperature conversion gained and water in tempering tank behind the mixing preparation with being pumped to tubular reactor, mixed solution and gaseous ammonia carry out neutralization reaction in tubular reactor, reaction back slip is delivered to spray-drying tower, spray in the drying tower by cat head, carry out vacuum flashing, at this moment Pen Wu fine silt in the landing process with the heat exchange of freezing air counter current contact and the cooling drying that rise; The product that falls at the bottom of the tower is delivered to the sieve apparatus screening through rotary conveyor, and the big pellet that sieves out is sent rotary conveyor back to by chapelet after crusher in crushing.The satisfactory qualified powdered granulated potassium ammonium sulfate of fineness degree is submitted to product outlet by the finished product lift, send packing department packing after, warehouse-in is the ammonium-potassium sulfate product.Because gas velocity is lower in present method process using self-heating drying mode, tower, the tail gas dustiness is few, only needs to wash in aiutage to get final product emptying; Washings is with the recycle pump absorption that circulate between aiutage and rinse bath, and behind additional a certain amount of clear water, circulation certain phase, these washing water can return to tempering tank and reuse.
By as seen above-mentioned, the manufacture method production technique of powdered granulated potassium ammonium sulfate of the present invention is simple, reduced investment, can widen the range of product of the S-based compound fertilizer factory of existing domestic employing low temperature conversion technology, increase the no chlorine sylvite raw material sources of the fertile secondary processing of compound enterprise, reduce the secondary processing expense of composite fertilizer.
Description of drawings
Fig. 1 is the technological process of production synoptic diagram when adopting powdered granulated potassium ammonium sulfate manufacture method of the present invention.
Number in the figure is: the inlet of 1-water; The inlet of 2-sal enixum; The 3-tubular reactor; The 4-rinse bath; The 5-recycle pump; The 6-sieve apparatus; The 7-product outlet; 8-finished product lift; The 9-crusher; The 10-chapelet; The 11-rotary conveyor; The 12-spray-drying tower; The 13-pump; The 14-tempering tank; 15-gaseous ammonia buffer tank; The 16-vaporizer; 17-liquefied ammonia inlet.
Embodiment
Below by embodiment the present invention is further described in detail, but the present invention is in no way limited to these embodiment.
Described these embodiment all adopt technical process as shown in Figure 1.Therefore, at first see also Fig. 1.Technological principle is as follows: change into gaseous ammonia from liquefied ammonia inlet 17 liquefied ammonia that enter by vaporizer 16, send into gaseous ammonia buffer tank 15 and deliver to tubular reactor 3 after metering; In addition, the potassium hydrogen sulfate solution of sulfuric acid and Repone K low temperature conversion gained and water enter tempering tank 14 (comprising the washings that returns) through sal enixum inlet 2 and water inlet 1 respectively, in tempering tank 14, deliver to tubular reactor 3 with pump 13 behind the mixing preparation, mixed solution and gaseous ammonia carry out neutralization reaction in tubular reactor 3, reaction back slip is delivered to spray-drying tower 12, spray in the drying tower 12 by cat head, carry out vacuum flashing, at this moment Pen Wu fine silt in the landing process with the heat exchange of freezing air counter current contact and the cooling drying that rise; The product that falls at the bottom of the tower is delivered to sieve apparatus 6 screenings through rotary conveyor 11, and the macrobead pellet that sieves out is sent rotary conveyor 10 back to by chapelet after crusher 9 is broken.The satisfactory qualified powdered granulated potassium ammonium sulfate of fineness degree is submitted to product outlet 7 by finished product lift 8 and discharges, send the packing department packing after, warehouse-in is the ammonium-potassium sulfate product.In this flow process,, only need in aiutage, to wash to get final product emptying because of the tail gas dustiness is low few; Washings, is circulated to certain phase and can returns to tempering tank 14 repeated uses behind additional a certain amount of clear water with recycle pump 13 absorptions that circulate between aiutage and rinse bath.
Embodiment 1
With 0.85 ton of sulfuric acid and Repone K low temperature conversion gained potassium hydrogen sulfate solution, water mixes in tempering tank for 0.5 ton, and mixed solution carries out neutralization reaction with 0.23 ton of gaseous ammonia in tubular reactor, and temperature is about 152 ℃ in the tubular reactor, the about 0.30MPa of pressure, the pH value of reaction back slip is about 4.5.The slip that comes out from tubular reactor sprays the drying tower in the spraying drying column overhead, vacuum flashing, the fine silt of spraying in the landing process with the freezing air contact heat-exchanging and the cooling drying that rise, the product that falls at the bottom of the tower is the ammonium-potassium sulfate product through screening, packing, and this product contains N 10.5%, K
2O18.5%, H
2O＜4%; The particle of granularity＜1mm＞90% (above-mentioned percentage is all in " quality ", down together).
With 0.89 ton of sulfuric acid and Repone K low temperature conversion gained potassium hydrogen sulfate solution, water mixes in tempering tank for 0.62 ton, and mixed solution carries out neutralization reaction with 0.25 ton of gaseous ammonia in tubular reactor, and temperature is about 145 ℃ in the tubular reactor, the about 0.35MPa of pressure, the pH value of reaction back slip is about 4.8.All the other operation stepss are with embodiment 1.The analytical results of this product is N 11.5%, K
2O 17.5%, H
2O＜4%; The particle of granularity＜1mm＞90%.
With 0.78 ton of sulfuric acid and Repone K low temperature conversion gained potassium hydrogen sulfate solution, water mixes in tempering tank for 0.25 ton, and mixed solution carries out neutralization reaction with 0.2 ton of gaseous ammonia in tubular reactor, and temperature is about 158 ℃ in the tubular reactor, the about 0.25MPa of pressure, the pH value of reaction back slip is about 4.2.All the other operation stepss are with embodiment 1.The analytical results of this product is N 9.8%, K
2O 19.5%, H
2O＜4%; The particle of granularity＜1mm＞90%.
Claims (3)
1. the manufacture method of a powdered granulated potassium ammonium sulfate compound fertilizer mainly is a neutralization reaction of utilizing sal enixum and ammonia, it is characterized in that, this compound manure manufacture method comprises the steps:
(1) being mixed and made into density with the potassium hydrogen sulfate solution that contains excess sulfuric acid and a small amount of unreacted Repone K of sulfuric acid and Repone K low temperature conversion gained and a certain amount of water is 1.58～1.62g/cm
3, temperature is 90～110 ℃ mixed slurry;
(2) mixed slurry carries out neutralization reaction with gaseous ammonia in tubular reactor, 140～160 ℃ of temperature of reaction, and pressure is 0.2～0.4MPa, the pH value of reaction back slip is 4～5;
(3) in the tubular reactor in and slip spray the drying tower from the spraying drying column overhead, in and slip in moisture content be depressurized flash distillation, the fine silt of spraying in the landing process with the freezing air contact heat-exchanging and the cooling drying that rise, at the bottom of tower, obtain the ammonium-potassium sulfate compound manure.
2. the manufacture method of powdered granulated potassium ammonium sulfate compound fertilizer according to claim 1 is characterized in that, adds the ratio of the water in the potassium hydrogen sulfate solution, in mass, is 0.3～0.7: 1.
3. the manufacture method of powdered granulated potassium ammonium sulfate compound fertilizer according to claim 1 is characterized in that, the add-on of gaseous ammonia is controlled according to the degree of neutralization of potassium hydrogen sulfate solution in the tubular reactor.
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| CN2006101472630A CN101200392B (en) | 2006-12-14 | 2006-12-14 | Method for manufacturing powdered granulated potassium ammonium sulfate compound fertilizer |
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| CN101200392B true CN101200392B (en) | 2010-12-15 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101423433B (en) * | 2008-11-27 | 2011-05-18 | 中国-阿拉伯化肥有限公司 | Method for preparing circular granule nitrogen and potassium fertilizer |
| CN103044167B (en) * | 2013-01-05 | 2014-04-16 | 中化山东肥业有限公司 | Technology for producing organic chelating polyelement compound fertilizer through guniting |
| CN103044157B (en) * | 2013-01-24 | 2014-05-07 | 山东红日阿康化工股份有限公司 | Amino acid guniting compound fertilizer and preparation method thereof |
| CN106268198A (en) * | 2016-07-27 | 2017-01-04 | 山东大学 | A kind of desulfurization fume dehumidifying and water reclamation system and method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045388A (en) * | 1989-03-10 | 1990-09-19 | 李换位 | Make the method for potassiumphosphate and NPK fertilizers at low temperatures by Repone K |
| CN1280967A (en) * | 2000-08-29 | 2001-01-24 | 陈爱中 | Process for preparing powdered composite potassium sulfate fertilizer |
| RU2230051C1 (en) * | 2003-05-27 | 2004-06-10 | Открытое Акционерное Общество "Научно-Исследовательский Институт По Удобрениям И Инсектофунгицидам Им. Проф. Я.В. Самойлова" | Method for preparing complex fertilizers |
| CN1844059A (en) * | 2006-03-24 | 2006-10-11 | 宜兴申利化工有限公司 | Method for preparing composite fertilizer of potassium sulfate and ammonium |
-
2006
- 2006-12-14 CN CN2006101472630A patent/CN101200392B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045388A (en) * | 1989-03-10 | 1990-09-19 | 李换位 | Make the method for potassiumphosphate and NPK fertilizers at low temperatures by Repone K |
| CN1280967A (en) * | 2000-08-29 | 2001-01-24 | 陈爱中 | Process for preparing powdered composite potassium sulfate fertilizer |
| RU2230051C1 (en) * | 2003-05-27 | 2004-06-10 | Открытое Акционерное Общество "Научно-Исследовательский Институт По Удобрениям И Инсектофунгицидам Им. Проф. Я.В. Самойлова" | Method for preparing complex fertilizers |
| CN1844059A (en) * | 2006-03-24 | 2006-10-11 | 宜兴申利化工有限公司 | Method for preparing composite fertilizer of potassium sulfate and ammonium |
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Address after: 200062 Shanghai Yunling Road No. 345 Patentee after: Shanghai Chemical Research Institute Co., Ltd. Address before: 200062 Shanghai Yunling Road No. 345 Patentee before: Shanghai Research Institute of Chemical Industry |
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