CN1042216C - Enriching slurry process for production of diammonium phosphate - Google Patents

Enriching slurry process for production of diammonium phosphate Download PDF

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Publication number
CN1042216C
CN1042216C CN92106621A CN92106621A CN1042216C CN 1042216 C CN1042216 C CN 1042216C CN 92106621 A CN92106621 A CN 92106621A CN 92106621 A CN92106621 A CN 92106621A CN 1042216 C CN1042216 C CN 1042216C
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CN
China
Prior art keywords
neutralization
slip
diammonium phosphate
flashing chamber
carry out
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Expired - Fee Related
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CN92106621A
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Chinese (zh)
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CN1076680A (en
Inventor
邵伟光
李尚民
应建康
罗洪波
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LAIXI PHOSPHATE FERTILIZER FACTORY
Chengdu University of Science and Technology
Original Assignee
LAIXI PHOSPHATE FERTILIZER FACTORY
Chengdu University of Science and Technology
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Application filed by LAIXI PHOSPHATE FERTILIZER FACTORY, Chengdu University of Science and Technology filed Critical LAIXI PHOSPHATE FERTILIZER FACTORY
Priority to CN92106621A priority Critical patent/CN1042216C/en
Publication of CN1076680A publication Critical patent/CN1076680A/en
Application granted granted Critical
Publication of CN1042216C publication Critical patent/CN1042216C/en
Anticipated expiration legal-status Critical
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05BPHOSPHATIC FERTILISERS
    • C05B7/00Fertilisers based essentially on alkali or ammonium orthophosphates

Abstract

The present invention provides a process for producing diammonium phosphate by a slurry concentration method. A neutralization tank is added behind an I-efficiency flash chamber in the existing process for producing monoammonium phosphate by a slurry concentration method to carry out secondary neutralization reaction with adding ammonium, and the neutralization degree of the slurry is improved to be 1.5 to 1.8 from 1.1 to 1.2. Thus, the diammonium phosphate according with a GB10205-88 national standard is produced.

Description

A kind of production method of diammonium phosphate
The present invention is the production method of enriching slurry method production diammonium phosphate.
At present, domestic production phosphorus ammonium mainly contains concentrated phosphoric acid method (traditional method) and two kinds of technologies of enriching slurry method.
The technical process of concentrated phosphoric acid method production diammonium phosphate is: with reference to Fig. 1, through the phosphoric acid (50-52%P after concentrating 2O 5) with after waste water from tail gas absorber mixes, enter in the neutralizing well 8 with gas ammonia through metering and carry out the neutralization reaction first time, degree of neutralization (mol ratio of ammonia and phosphoric acid) is controlled at 1.4-1.5, slurry temperature 120-125 ℃.Enter ammonification again with slip in generating---in the tablets press 15; add liquefied ammonia and returning charge simultaneously; make phosphoric acid and liquefied ammonia carry out the neutralization reaction second time; and carry out granulation; the granulous diammonium phosphate enters in the drying cylinder 16 with temperature 180-200 ℃ hot gas carrier carries out and fluidized drying; dried product sieves, the unlap after air-cooled of qualified particle.The concentrated phosphoric acid method can the production diammonium phosphate, but must use P 2O 5Content is higher than 30%, iron, aluminium, Rock Phosphate (72Min BPL) that magnesium addition content is low are produced, and the material of equipment is had relatively high expectations.If with in, low grade ore production because impurity is many, easily fouling is difficult in concentration process removes for complex compounds such as iron, aluminium, magnesium, makes production can not carry out (even can't carry out) smoothly, the low (20-25%P of the phosphoric acid concentration of generation 2O 5), viscosity is big, and it is big to concentrate load, can't reach throughput.
The technical process that the enriching slurry method is produced monoammonium phosphate is: with reference to Fig. 2, the dilute phosphoric acid that is come by the washing lotion circulation groove enters in the downtake of II effect flashing chamber 3 after metering, imitate recycle pump 6 through II and enter II effect well heater 5, in the feed slurry inlet pipe of II effect flashing chamber 3, feed ammonia, make phosphoric acid and gas ammonia in this pipe, neutralization reaction take place, degree of neutralization is controlled at 1.1-1.2, enters II effect flashing chamber 3 with slip in the formation and concentrates.Meanwhile, imitate in II under the effect of recycle pump 6, slip in the II effect flashing chamber 3 is along adding dilute phosphoric acid again in the downtake decline process, react with gas ammonia again after heater via 5 heating, enter II and imitate flashing chamber 3 and concentrate, so move in circles, neutralize constantly, concentrate that (it is concentration integrated that this technology is called neutralization, be present state-of-the-art technology, apply for national inventing patent between 1991 9, October) by Chengdu Univ. of Science ﹠ Technology.II is imitated II after neutralization concentrates in the flashing chamber 3 and is imitated slip and send to I through punishment in advance pump 7 and imitate flashing chamber 4 and carry out further concentrating, and makes slip moisture content be controlled at 25-32%.I is imitated and is used the live steam heating, and concentration process is identical with the II effect, and I is imitated slip (terminal point slip) and overflowed to slip dashpot 9, delivers to spray granulation drier 10 by spray pump and carries out granulation, drying.The secondary steam that I is imitated generation goes II effect well heater 5 to make thermal source, and the secondary steam that II is imitated generation goes mixing condenser 1 condensation, discharges non-condensable gases, makes the required vacuum tightness 0.05-0.06MP of II effect flashing chamber 3 maintenances aIt is more advanced that the enriching slurry method is produced phosphorus ammonium technology, require low to ore, but its shortcoming is can only produce monoammonium phosphate and can not the production diammonium phosphate, reason is that the slip after once neutralizing enters II flashing chamber 3 and I and imitates in the flashing chamber 4 and concentrate, because I is imitated the big (0.05-0.06MP of vacuum tightness that temperature higher (120-125 ℃) in the flashing chamber 4, II are imitated flashing chamber 3 a), with this understanding, degree of neutralization is when 1.1-1.2, and ammonia loses less than 1%, but when degree of neutralization greater than 1.2 the time, the loss of ammonia sharply increases, after slip entered I effect flashing chamber 4 by II effect flashing chamber 3, the ammonia of adding is complete loss almost, and final degree of neutralization can only be 1.1-1.2, degree of neutralization can't improve again, must reach 1.5-1.8 and will produce qualified diammonium phosphate slurry degree of neutralization.
Task of the present invention is to improve enriching slurry method monoammonium phosphate production technique, improves the slip degree of neutralization, produces the diammonium phosphate that meets the GB10205-88 national standard.
Task of the present invention is finished as follows: it is characterized in that this method takes following steps:
A, dilute phosphoric acid and gas ammonia carry out neutralization reaction one time in II is imitated the recycle system that flashing chamber, recycle pump and well heater constitute, just degree of neutralization reaches 1.1-1.2;
Slip after b, the neutralization enters I through the punishment in advance pump and imitates flashing chamber, circulates concentrated with the live steam that adds in I is imitated the recycle system that flashing chamber, recycle pump and well heater constituted;
C, the slip after concentrating overflows to neutralizing well and gas ammonia carries out the secondary neutralization reaction, makes degree of neutralization bring up to 1.5-1.8, and the neutralizing well slurry temperature is at 100-110 ℃, about 45 minutes of required time;
D, the slip after the secondary neutralization reaction overflow to slip and give in the dashpot, deliver to spray granulation drier again and carry out granulation, drying, deliver to vibratory screening apparatus by bucket elevator and sieve, and the qualified diammonium phosphate grain that sieves out removes finished product packing.
Advantage of the present invention and positively effect are: owing to set up fourth secondary neutralization reaction operation, improved the slip degree of neutralization, the production through 6 months proves that product meets GB10205-88 diammonium phosphate technological standard, and nitrogen content 〉=13% reaches as high as 16%, P 2O 5Content (EDTA dissolubility phosphorus) can reach 42-46%.
The present invention is described in further detail below in conjunction with accompanying drawing:
Fig. 1 is a concentrated phosphoric acid method production diammonium phosphate process flow sheet.
Fig. 2 is that the enriching slurry method is produced the monoammonium phosphate process flow sheet.
Fig. 3 is the process flow sheet of enriching slurry production diammonium phosphate of the present invention.
Wherein 1 is mixing condenser, the 2nd, and liquid seal trough, the 3rd, II is imitated flashing chamber; the 4th, I is imitated flashing chamber, 5,5 ' be well heater, 6,6 ' be recycle pump; the 7th, punishment in advance pump, the 8th, neutralizing well (secondary ammonification), the 9th, slip dashpot; the 10th, material dryer is made in whitewashing, and the 11st, bucket elevator, the 12nd, vibratory screening apparatus; the 13rd, crusher; the 14th, return conveyer machine, the 15th, ammonification one tablets press, the 16th, drying cylinder.
Referring to Fig. 3, be the example explanation to produce 30000 tons of diammonium phosphate per year.By the next dilute phosphoric acid (22%P of washing lotion circulation groove 2O 5) enter in the downtake that II imitates flashing chamber 3 with 9390 kilograms flow per hour, pump into well heater 5 by recycle pump 6 again, the gas ammonia that is come by the ammonia station enters in the feed slurry inlet pipe that II imitates flashing chamber 3 with 559.6 kilograms flow per hour, phosphoric acid and gas ammonia carry out a neutralization reaction (3.5 meters of pipe ranges) in this pipe, entering II effect flashing chamber 3 then concentrates, meanwhile, slip mixes with the dilute phosphoric acid of adding after recycle pump 6 enters well heater 5 heating through downtake again, entering II effect flashing chamber 3 after reacting with the gas ammonia that adds concentrates again, move in circles, it is concentrated to finish once neutralization, makes degree of neutralization reach 1.1-1.2, and slip moisture content reaches 40-50%.II imitate slip by punishment in advance pump 7 with 9386.2 kilograms flow per hour deliver to I imitate flashing chamber 4, I imitate well heater 5 ', heat with live steam, recycle pump 6 ' effect under, circulation concentrates, make slip moisture content drop to 30% (concentration process is imitated identical with II), overflow to neutralizing well 8 again and carry out secondary neutralization reaction (design stopped 45 minutes, interior slurry temperature 100-110 ℃ of neutralizing well), make degree of neutralization bring up to 1.5-1.8 by 1.1-1.2 with the gas ammonia that per hour adds 100 kilograms.Slip after the secondary neutralization reaction overflows in the slip dashpot 9, and moisture content is reduced to about 25%, delivers to spray granulation drier 10 again and carries out granulating and drying.Afterwards, sieved by vibratory screening apparatus 12, qualified particle of small portion and fine powder are done returning charge, and oversize material is done returning charge after crusher 13 fragmentations, and most of qualified particle removes finished product packing.Equipment used of the present invention is produced monoammonium phosphate equipment with the enriching slurry method, only needs to increase a corresponding volumetrical neutralizing well, other Working Procedure Controlling parameter constant.

Claims (1)

1, a kind of production method of diammonium phosphate is characterized in that this method takes following steps:
A, dilute phosphoric acid and gas ammonia carry out neutralization reaction one time in II is imitated the recycle system that flashing chamber (3), recycle pump (6) and well heater (5) constituted, make degree of neutralization reach 1.1-1.2;
Slip after b, the neutralization enters I through punishment in advance pump (7) and imitates flashing chamber (4), circulates concentrated with the live steam that adds in the recycle system that I effect flashing chamber (4), recycle pump (6 ') and well heater (5 ') are constituted;
C, the slip after concentrating overflow to neutralizing well (8) and carry out the secondary neutralization reaction with gas ammonia, make degree of neutralization bring up to 1.5-1.8, and neutralizing well (8) slurry temperature is at 100-110 ℃, about 45 minutes of required time;
D, the slip after the secondary neutralization reaction overflow in the slip dashpot (9), deliver to spray granulation drier (10) again and carry out granulation, drying, deliver to vibratory screening apparatus (12) by bucket elevator (11) and sieve, the qualified diammonium phosphate grain that sieves out removes finished product packing.
CN92106621A 1992-07-17 1992-07-17 Enriching slurry process for production of diammonium phosphate Expired - Fee Related CN1042216C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN92106621A CN1042216C (en) 1992-07-17 1992-07-17 Enriching slurry process for production of diammonium phosphate

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Application Number Priority Date Filing Date Title
CN92106621A CN1042216C (en) 1992-07-17 1992-07-17 Enriching slurry process for production of diammonium phosphate

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CN1076680A CN1076680A (en) 1993-09-29
CN1042216C true CN1042216C (en) 1999-02-24

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1309658C (en) * 2003-10-24 2007-04-11 四川大学 Method of processing waste gas from ammonium phosphate plate into slurry for two-purpose utilization

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1084316C (en) * 1999-01-15 2002-05-08 安徽六国化工股份有限公司 Method and apparatus for producing diammonium phosphate with external circulation ammoniation reactor
CN100371238C (en) * 2006-06-16 2008-02-27 四川川大中德环保技术有限公司 Method for producing diammonium phosphate by concentrating acid slime, and secondary ammoniation reactor
CN100441502C (en) * 2006-08-24 2008-12-10 四川川大中德环保技术有限公司 Method of classification utilizing wet-process phosphoric acid
CN101857210B (en) * 2010-06-04 2012-02-15 广西钦州桂金诺磷化工有限公司 Method for producing industrial grade diammonium phosphate from wet-process phosphoric acid
CN102086131A (en) * 2010-11-23 2011-06-08 瓮福(集团)有限责任公司 Method for co-producing diammonium phosphate by powdery monoammonium phosphate production device
CN102807200B (en) * 2011-06-03 2014-07-30 马叔骥 Method for preparing full-water-soluble efficient compound fertilizer ammonium phosphate from industrial-quality phosphoric acid
CN103011112A (en) * 2012-12-12 2013-04-03 瓮福(集团)有限责任公司 Production method of diammonium phosphate product
CN103395762B (en) * 2013-08-17 2016-03-16 威海恒邦化工有限公司 A kind of phosphorus ammonium produce in the concentration method of slip and device
CN104888482A (en) * 2015-05-13 2015-09-09 江苏瑞和化肥有限公司 Double-effect evaporation final-effect vapour system
CN107200315B (en) * 2017-06-28 2023-07-21 四川省高宇化工有限公司 Method and device for producing monoammonium phosphate based on multi-neutralization wet-process phosphoric acid
CN111423272A (en) * 2020-03-31 2020-07-17 湖北万丰化工有限公司 Method for producing fertilizer by slurry method

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US351425A (en) * 1886-10-26 Vehicle-axle
CA122236A (en) * 1909-10-29 1909-11-30 Howard P. Davies Nut-lock
SU152005A1 (en) * 1961-11-24 1961-11-30 Ю.М. Гельфгат Hydraulic converter to a device for soldering and tinning printed circuit boards
EP0161704A2 (en) * 1984-04-18 1985-11-21 ENICHEM AGRICOLTURA S.p.A. Process for the production of water soluble ammonium phosphates
CN1055912A (en) * 1988-11-08 1991-11-06 挪威海德罗公司 The method for preparing granulated di-ammonium phosphate containing fertilizer

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US351425A (en) * 1886-10-26 Vehicle-axle
CA122236A (en) * 1909-10-29 1909-11-30 Howard P. Davies Nut-lock
SU152005A1 (en) * 1961-11-24 1961-11-30 Ю.М. Гельфгат Hydraulic converter to a device for soldering and tinning printed circuit boards
EP0161704A2 (en) * 1984-04-18 1985-11-21 ENICHEM AGRICOLTURA S.p.A. Process for the production of water soluble ammonium phosphates
CN1055912A (en) * 1988-11-08 1991-11-06 挪威海德罗公司 The method for preparing granulated di-ammonium phosphate containing fertilizer

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Title
磷肥与复肥 1989.1.1 张允湘,料浆法磷铵技术讲座第二讲湿法 磷酸的氨中和 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1309658C (en) * 2003-10-24 2007-04-11 四川大学 Method of processing waste gas from ammonium phosphate plate into slurry for two-purpose utilization

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