CN1336354A - Production process of sulfur-base composite azophoska - Google Patents

Production process of sulfur-base composite azophoska Download PDF

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Publication number
CN1336354A
CN1336354A CN 00122413 CN00122413A CN1336354A CN 1336354 A CN1336354 A CN 1336354A CN 00122413 CN00122413 CN 00122413 CN 00122413 A CN00122413 A CN 00122413A CN 1336354 A CN1336354 A CN 1336354A
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China
Prior art keywords
phosphorus
controlled
nitration mixture
reaction
qualified
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CN 00122413
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Chinese (zh)
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刘远明
李晓东
李旭修
刘文俊
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QINGDAO CHANGHUA GROUP CORP
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QINGDAO CHANGHUA GROUP CORP
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Priority to CN 00122413 priority Critical patent/CN1336354A/en
Publication of CN1336354A publication Critical patent/CN1336354A/en
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Abstract

The present invention relates to production method of sulfur base nitrogen phosphorus potassium composite fertilizer, it is prepared through regulating the proportion of mineral slurry in acid hydrolysis reaction kettle to produce phosphoric acid with different P2O5 ratio and through the reaction of potassium hydrogen sulfate to produce mixed acid, then the mixed acid is neutralized with gaseous ammonia, finally spray dried and pellatized to produce 25-40% sulfur base nitrogen phosphorus potassium complex fertilizer with rarious nutrition ratio. Said method does not discharge phosphogypsum and is low in production cost.

Description

A kind of production method of sulfenyl nitrogen-phosphorus-potassium compound fertilizer
The present invention relates to a kind of production method of sulfenyl nitrogen-phosphorus-potassium compound fertilizer, especially relate to the production method that a kind of low temperature conversion method is produced sulfenyl nitrogen-phosphorus-potassium compound fertilizer.
At present, the production method of sulfenyl nitrogen-phosphorus-potassium compound fertilizer mainly is a slurry process, produces in the sulfenyl nitrogen-phosphorus-potassium compound fertilizer at slurry process, can be divided into spray granulating method and drum granulating method according to granulation mode difference, if K 2O changes into sal enixum at low temperatures by Repone K, then is the low temperature slurry process; If K 2O is directly provided by vitriolate of tartar and then is traditional slurry process.
It is to adopt to contain greater than 45%P that the tradition slurry process is produced sulfenyl nitrogen-phosphorus-potassium compound fertilizer 2O 5Phosphoric acid and ammonia in groove type reactor or tubular reactor, carry out neutralization reaction; produce phosphor ammonium slurry; vitriolate of tartar and insufficient nitrogen are all brought granulating system into from returning charge; in tablets press, mix the back granulation with slip; physical process such as drying, screening, fragmentation obtain the granular sulfenyl nitrogen-phosphorus-potassium compound fertilizer of finished product again; this production method is suitable for large-scale fertilizer factory, and outside returns is adopted in the returning charge of granulation process, and investment is big.
It is sulfuric acid and Repone K massage to be shown than about 1: 1 ℃-140 ℃ fully react the 20%-22%P that contains that removes phosphogypsum after filtration of the potassium hydrogen sulfate solution of production and phosphoric acid workshop section with steam heating to 110 in reactive tank that the low temperature slurry process is produced sulfenyl nitrogen-phosphorus-potassium compound fertilizer 2O 5Dilute phosphoric acid mix, generate nitration mixture (proportion 1.40-1.45), with being pumped to tubular reactor and carrying out neutralization reaction from the gas ammonia (0.2-0.3MPa) at ammonia station, degree of neutralization is controlled between the 1.2-1.3, make the water content of slip be controlled at 25-35%,, carried out drying by warm air from hotblast stove with being pumped to spray granulation drier, dry back product sieves, the unlap after air-cooled of qualified particle.Can only produce the sulfenyl nitrogen-phosphorus-potassium compound fertilizer material (nutrient consists of 12-18-15) of 45% nutrient with this method, and will the composite fertilizer of production nutrient content between 25%-40%, need in the tablets press interpolation phosphogypsum as a supplement.Like this, needing on the one hand increases necessary equipment and manpower, causes cost to rise, and on the other hand, phosphoric acid production is discharged a large amount of phosphogypsums, need take a large amount of land resources, and serious environment pollution.
Task of the present invention provides a kind of production method of sulfenyl nitrogen-phosphorus-potassium compound fertilizer, makes in the production of sulfenyl nitrogen-phosphorus-potassium compound fertilizer, and the phosphogypsum of phosphoric acid workshop section does not efflux, and can produce from the sulfenyl nitrogen-phosphorus-potassium compound fertilizer of the various nutrient ratios of 25%-40%.
Task of the present invention is finished as follows: it is characterized in that this method takes following steps:
A. the phosphorus ore for preparing is through fragmentation, grinding, density measurement, after qualified, deliver to the phosphorus ore acid hydrolysis reactive tank and the vitriol oil reacts by shurry pump, temperature of reaction is controlled between 65-80 ℃, liquid phase in the slip (phosphoric acid solution) is 3-3.5 to the mass ratio of solid phase (phosphogypsum): 1, and make qualified ore pulp (without a series of equipment such as filters) and deliver to the nitration mixture groove;
B. the Repone K and the vitriol oil react in being provided with the reactive tank of agitator, temperature of reaction is controlled at 110 ℃-130 ℃, reaction times was controlled at 1.5-2 hour, and the mol ratio of sulfuric acid and Repone K is controlled between the 1-1.2, and the potassium hydrogen sulfate solution of production mixes with ore pulp in the nitration mixture groove and generates nitration mixture;
C. nitration mixture and gas ammonia after metering carry out neutralization reaction in tubular reactor, and the gained slip carries out granulation, drying through spray granulation drier, sends into roto-sifter by bucket elevator and sieves, and the qualified particle that sieves out removes finished product packing through cooling.
Advantage of the present invention and positively effect are: technical process short (phosphoric acid workshop section has saved a series of equipment such as filter), save electric energy, and product cost is low, and no phosphogypsum discharging can be produced from the composite fertilizer of the various nutrient ratios of 25-40%.
Below in conjunction with accompanying drawing the present invention is described in further detail.
Fig. 1 is that low temperature conversion method of the present invention is produced sulfenyl nitrogen-phosphorus-potassium compound fertilizer phosphoric acid workshop section process flow sheet;
Fig. 2 is that low temperature conversion method of the present invention is produced sulfenyl nitrogen-phosphorus-potassium compound fertilizer conversion workshop section process flow sheet;
Fig. 8 is that low temperature conversion method of the present invention is produced sulfenyl nitrogen-phosphorus-potassium compound fertilizer composite fertilizer workshop section process flow sheet.
Wherein 1 is the sulphur acid meter measuring tank, the 2nd, and sulfuric acid pump, the 3rd, gas blower, the 4th, shurry pump, the 5th, acidolysis reaction groove, the 6th, fluorine absorbent recirculation pump, the 7th, Venturi absorption tower, the 8th, exhaust blower, the 9th, aiutage, the 10th, lift, the 11st, feed bin, the 12nd, metering screw, the 13rd, feed spiral, the 14th, reactive tank, the 15th, sulphuric acid tank, the 16th, magnetic flow meter, the 17th, nitration mixture groove, the 18th, nitration mixture pump, the 19th, tubular reactor, the 20th, neutralizing well, the 21st, sloptank, the 22nd, hotblast stove, the 23rd, spray granulation drier, the 24th, roto-sifter, the 25th, crusher, the 26th, returning charge worm conveyor.
With reference to Fig. 1, Fig. 2, Fig. 3, be the example explanation to produce 100000 ton of 30% sulfenyl nitrogen-phosphorus-potassium compound fertilizer per year.The phosphorus ore for preparing enters ball mill grinding through broken, weighing with 4.5 tons speed per hour, mill ore pulp well is through density measurement, after qualified, flow into the ore pulp storage tank, deliver to the phosphorus ore acid hydrolysis reactive tank and per hour measure 98% dense H of 4578Kg flow through magnetic flow meter through magnetic flow meter by pump 2SO 4React, temperature of reaction is controlled between 65-80 ℃, and the mass ratio of liquid phase and solid phase is 3-3.5 in the slip: 1, and make qualified ore pulp and (contain 15-16%P 2O 5) deliver to nitration mixture groove 18, Repone K is sent into reactive tank 14 with the speed of 2158kg per hour and is generated sal enixum with 98% the strong sulfuric acid response of sending into reactive tank 14 with 3122 kilograms flow velocity per hour, the sal enixum that generates overflows to nitration mixture groove 17, mix with the phosphoric acid ore pulp in the nitration mixture groove 17, make its specific gravity control between 1.35-1.45, be pumped to tubular reactor 19 by composite fertilizer workshop section then, with per hour flow from the ammonia station be that 1820 kilograms gas ammonia carries out neutralization reaction, its degree of neutralization is controlled between the 1.0-1.3, slip enters neutralizing well 20, moisture content is through sharply evaporation, between the last slip water content control 25%-35%, slip overflows to sloptank 21 by neutralizing well 20, be driven into spray granulation drier 23 by pump then, mix from spray gun with the pressurized air of 0.2-0.3MPa and to spray, slip is sprayed on the material curtain of spray granulation drier 23 and carries out coating granulation, warm air (450 ℃-550 ℃) from hotblast stove 22 passes through the material curtain, material is carried out and fluidized drying, material carries out internal return in spray granulation drier 23, composite fertilizer sends into roto-sifter 24 for bucket elevator 10 after dry, after screening, particle greater than 4mm enters crusher 25, broken back enters returning charge worm conveyor 26 less than particle and the dust of 1mm, qualified particle enters cooler, below air cooling to 40 ℃, product is delivered to finished bin with 14000 kilograms flow per hour by the belt lift, through metering, stack packing back, and the steam that spray granulation drier 23 produces and the warm air of the cooler gas dust-removal system that truncates is handled.
Produce 25% sulfenyl nitrogen-phosphorus-potassium compound fertilizer, only need P ore pulp in the acidolysis reaction groove 2O 5Content is controlled between the 8%-12%, and all the other technic indexs are with producing 30% sulfenyl nitrogen-phosphorus-potassium compound fertilizer.
Produce 40% sulfenyl nitrogen-phosphorus-potassium compound fertilizer, only need in the sloptank 21 of composite fertilizer workshop section, to add the monoammonium phosphate of some amount, add 20-26 part (weight part) monoammonium phosphate in per 100 parts of (weight part) slips, all the other technic indexs are with producing 30% sulfenyl nitrogen-phosphorus-potassium compound fertilizer.
Equipment used of the present invention is produced sulfenyl nitrogen-phosphorus-potassium compound fertilizer equipment similar in appearance to the low temperature conversion method, just saves a series of equipment such as filter in phosphoric acid workshop section, and other Working Procedure Controlling parameter is identical.

Claims (1)

1, a kind of production method of sulfenyl nitrogen-phosphorus-potassium compound fertilizer is characterized in that this method takes following steps:
A. the phosphorus ore for preparing is through fragmentation, grinding, density measurement, after qualified, delivering to phosphorus ore acid hydrolysis reactive tank (5) by shurry pump reacts with the vitriol oil, temperature of reaction is controlled between 65-80 ℃, liquid phase is 3-3.5 to the mass ratio of solid phase in the slip: 1, and make qualified ore pulp and deliver to nitration mixture groove (17);
B. the Repone K and the vitriol oil react in being provided with the reactive tank of agitator (14), temperature of reaction is controlled at 110 ℃-130 ℃, reaction times was controlled at 1.5-2 hour, rubbing of sulfuric acid and Repone K is than being controlled between the 1-1.2, and the potassium hydrogen sulfate solution of production mixes with ore pulp in nitration mixture groove (17) and generates nitration mixture;
C. nitration mixture and the gas ammonia through measuring carry out neutralization reaction in tubular reactor (19), the gained slip is delivered to spray granulation drier (23) and is carried out granulation, drying, send into roto-sifter (24) by bucket elevator (10) and sieve, the qualified particle that sieves out removes finished product packing through cooling.
CN 00122413 2000-07-29 2000-07-29 Production process of sulfur-base composite azophoska Pending CN1336354A (en)

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Application Number Priority Date Filing Date Title
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100354235C (en) * 2006-04-06 2007-12-12 潍坊昌大肥料有限公司 Spray pelleting process of compound fertilizer
CN101284743B (en) * 2007-04-10 2012-02-22 上海化工研究院 Process for preparing complex fertilizer using sulfuric acid and ammine as partial raw material
CN102584408A (en) * 2012-03-23 2012-07-18 河北冀衡赛瑞化工有限公司 Method for producing nitro-sulfur-based composite fertilizer by full-liquid phase high tower granulation
CN101648829B (en) * 2009-08-20 2012-09-19 中国-***化肥有限公司 Highly integrated co-production method of nitrate-based compound fertilizer and chlorine base fertilizer
CN110483125A (en) * 2019-08-02 2019-11-22 史丹利化肥当阳有限公司 Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100354235C (en) * 2006-04-06 2007-12-12 潍坊昌大肥料有限公司 Spray pelleting process of compound fertilizer
CN101284743B (en) * 2007-04-10 2012-02-22 上海化工研究院 Process for preparing complex fertilizer using sulfuric acid and ammine as partial raw material
CN101648829B (en) * 2009-08-20 2012-09-19 中国-***化肥有限公司 Highly integrated co-production method of nitrate-based compound fertilizer and chlorine base fertilizer
CN102584408A (en) * 2012-03-23 2012-07-18 河北冀衡赛瑞化工有限公司 Method for producing nitro-sulfur-based composite fertilizer by full-liquid phase high tower granulation
CN102584408B (en) * 2012-03-23 2014-01-15 河北冀衡赛瑞化工有限公司 Method for producing nitro-sulfur-based composite fertilizer by full-liquid phase high tower granulation
CN110483125A (en) * 2019-08-02 2019-11-22 史丹利化肥当阳有限公司 Utilize the method for waste phosphoric acid production S-based compound fertilizer raw material
CN110483125B (en) * 2019-08-02 2022-03-04 史丹利化肥当阳有限公司 Method for producing raw material for sulfur-based compound fertilizer by using waste phosphoric acid

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