CN101891504B - Method for producing granular monoammonium phosphate with raffinate - Google Patents
Method for producing granular monoammonium phosphate with raffinate Download PDFInfo
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- CN101891504B CN101891504B CN2010102364964A CN201010236496A CN101891504B CN 101891504 B CN101891504 B CN 101891504B CN 2010102364964 A CN2010102364964 A CN 2010102364964A CN 201010236496 A CN201010236496 A CN 201010236496A CN 101891504 B CN101891504 B CN 101891504B
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- phosphoric acid
- raffinate
- monoammonium phosphate
- phosphate
- neutralization
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Abstract
The invention provides a method for producing granular monoammonium phosphate with raffinate, wherein, ammonia is neutralized with phosphoric acid to obtain slurry, and the slurry is concentrated and then subjected to spraying granulation to obtain the granular monoammonium phosphate. The method comprises the following steps: (1) mixing wet-process phosphoric acid with the raffinate according to a certain ratio to obtain mixed phosphoric acid, and then lowering the metal ion content in the raw material mixed phosphoric acid; and (2) adjusting the neutralization degree of neutralization reaction between the mixed phosphoric acid and the ammonia to obtain monoammonium phosphate slurry. The granular monoammonium phosphate obtained by the method can meet the requirement for nitrogen nutrients in the product, reach the product strength of no less than 40N, digest the raffinate in a wet-process phosphoric acid purification device, conform to the requirement for the current global recycling economy. The method can improve the concentration of dilute phosphoric acid, reduce steam consumption of a slurrying system, and increase the product strength of the granular monoammonium phosphate.
Description
[affiliated technical field]
The present invention relates to phosphate fertilizer, relate in particular to monoammonium phosphate, relate in particular to the method for the raffinate production granular monoammonium phosphate that utilizes purification of wet process phosphoric acid.
[background technology]
As everyone knows, the purification process of phosphoric acid by wet process has had new development in recent years, and the phosphoric acid by wet process quality after the purification can compare favourably with thermal phosphoric acid, and production cost is lower, and the trend that replaces thermal phosphoric acid is arranged at industrial circle.In the liquid-liquid solvent extraction method purification of wet process phosphoric acid flow process that generally adopts at present, can the by-product raffinate.Raffinate generally is used to make fertilizer.When using raffinate to produce fertilizer, because of F in the raffinate
-, SO
4 2-Reduce Deng anion-content, but enrichment the metallic cation in the phosphoric acid by wet process; Compare with common phosphoric acid by wet process, variation has taken place in the content of foreign ion, chemical fertilizer product total nitrogen content by its production often occurs and does not reach the problem that specification of quality or product moisture exceed standard.Along with the normal operation of wet phosphoric acid purifying device, raffinate constantly increases, can digest these raffinates become the wet phosphoric acid purifying device can the quantity-produced important factor in order.
At present, relate to the one Chinese patent application part that utilizes raffinate to produce phosphate fertilizer " with the method for the raffinate production diammonium phosphate of purifying phosphoric acid ", the application part of the monoammonium phosphate of the raffinate of useless purifying phosphoric acid production are still only arranged No. 200910102694.9.
[summary of the invention]
The objective of the invention is in order to digest raffinate; Guarantee that the wet phosphoric acid purifying device moves continuously; Product nitrogen contains quantity not sufficient and the problem that product moisture exceeds standard when solve using raffinate to produce ammophos simultaneously, and a kind of method of utilizing raffinate production granular monoammonium phosphate is provided.
The contriver is through discovering, raffinate is compared with phosphoric acid by wet process, and metal ion contents such as iron, aluminium, magnesium are higher, and anion-contents such as fluorine, sulfate radical are lower.Produce in the phosphorus ammonium flow process at slurry process, metals ions such as iron, aluminium, magnesium make phosphoric acid in the ammonia N-process, generate multiple complex compound, and they will influence phosphor ammonium slurry viscosity and ammonium phosphate product composition, rerum natura and P
2O
5Solvability.The increase of metals ion (especially magnesium) will make phosphor ammonium slurry viscosity become big, and the slip water cut after concentrating increases, and cause the extremely difficult control of product moisture content.Simultaneously, the product total nitrogen content is not enough, does not reach the quality product requirement.
Product situation such as the following table of using raffinate to produce granular MAP separately:
Table 1 raffinate quality situation
The granular MAP quality product situation that table 2 raffinate is produced
It is thus clear that: directly produce monoammonium phosphate with raffinate, because metal ion contents such as iron wherein, aluminium, magnesium are higher, and anion-contents such as fluorine, sulfate radical are lower.And the variation of impurity makes phosphor ammonium slurry viscosity become big, and the slip water cut after concentrating increases, and causes the extremely difficult control of product moisture content; Simultaneously, in phosphoric acid metal ion content more for a long time, the NH that the phosphor ammonium slurry degree of neutralization that acid records is actual
3/ H
3PO
4Mol ratio is higher, makes the N/P of product on the low side, causes the product total nitrogen content not enough, does not reach the quality product requirement, can not make the product total nitrogen satisfy specification of quality even heighten phosphoric acid ammonification degree of neutralization.
To the problems referred to above, the method that the contriver provides utilizes raffinate to produce granular monoammonium phosphate has following two main points: 1. with phosphoric acid by wet process and raffinate by a certain percentage proportioning be made into mixed phosphate, the metal ion content of reduction raw materials mix phosphoric acid; 2. adjust the degree of neutralization of mixed phosphate and ammonia neutralization reaction, make the monoammonium phosphate slip.
Concrete scheme is:
Adopt P earlier
2O
5Massfraction is about 40% raffinate and P
2O
5Massfraction be about 25% dilute phosphoric acid by 15～18: 1 carries out proportioning, reduces cations, obtains mixed phosphate; With this mixed phosphate of ammonia neutralization, the reaction slurry degree of neutralization is brought up to 1.05～1.25 by 0.95～1.02 of original control again, to increase the nitrogen content in the product; According to common process reaction slurry is concentrated afterwards, last spray granulating is processed granular monoammonium phosphate.
The granular monoammonium phosphate that adopts present method to produce can satisfy the requirement of product nitrogen nutrient; Product strength is not less than 40N; Digest the raffinate of wet phosphoric acid purifying device, met the requirement of world today's recycling economy, improved the concentration of dilute phosphoric acid; Reduce the steam consumption of pulping system, increased granular monoammonium phosphate product intensity.
[embodiment]
Embodiment:
Adopt the inventive method, promptly adopt P earlier
2O
5Massfraction is about 40% raffinate and P
2O
5Massfraction be about 25% dilute phosphoric acid by 15～18: 1 carries out proportioning, obtains complex acid; Use in the ammonia again and complex acid, the reaction slurry degree of neutralization is controlled to be 1.05～1.20; According to common process reaction slurry is concentrated afterwards, last spray granulating is processed granular monoammonium phosphate.
The raffinate quality situation that is used for complex acid
The wet method dilute phosphoric acid quality situation that is used for complex acid
Join quality situation with acid
The granular MAP quality product situation that complex acid is produced
Phosphoric acid ammonification degree of neutralization is controlled at 1.05～1.20.
Complex acid through with phosphoric acid by wet process and raffinate is regulated, and the metal ion content in the raw material complex acid has reduced, thereby has improved the rerum natura of monoammonium phosphate slip, is convenient to production control; Simultaneously, do not need excessively to improve phosphoric acid ammonification degree of neutralization, can make the product total nitrogen satisfy specification of quality.
Claims (2)
1. utilize raffinate to produce the method for granular monoammonium phosphate; Be to process slip with the ammonia neutralising phosphoric acid; Concentrate the back spray granulating and process granular monoammonium phosphate; Its characteristic comprises: 1. with phosphoric acid by wet process and raffinate by a certain percentage proportioning be made into mixed phosphate, reduce the metal ion content of raw materials mix phosphoric acid; Said mixed phosphate is to adopt P
2O
5Massfraction is 40% raffinate and P
2O
5Massfraction be 25% dilute phosphoric acid by 15～18: 1 carries out the mixed phosphate that proportioning obtains; 2. adjust the degree of neutralization of mixed phosphate and ammonia neutralization reaction, make the monoammonium phosphate slip.
2. the method for claim 1, the degree of neutralization that it is characterized in that said adjustment mixed phosphate and ammonia neutralization reaction is that the reaction slurry degree of neutralization is controlled to be 1.05～1.25.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102364964A CN101891504B (en) | 2010-07-26 | 2010-07-26 | Method for producing granular monoammonium phosphate with raffinate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102364964A CN101891504B (en) | 2010-07-26 | 2010-07-26 | Method for producing granular monoammonium phosphate with raffinate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101891504A CN101891504A (en) | 2010-11-24 |
| CN101891504B true CN101891504B (en) | 2012-07-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010102364964A Active CN101891504B (en) | 2010-07-26 | 2010-07-26 | Method for producing granular monoammonium phosphate with raffinate |
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Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102161602B (en) * | 2010-12-28 | 2014-01-15 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium compound fertilizer by utilizing raffinate and phosphate tailings with high magnesium content |
| CN102020257B (en) * | 2010-12-31 | 2012-08-22 | 甘肃瓮福化工有限责任公司 | New technology of applying double-effect forced circulation concentration method in production of ammonium phosphate |
| CN102431985A (en) * | 2011-10-18 | 2012-05-02 | 瓮福（集团）有限责任公司 | Device for producing powdery monoammonium phosphate by using extraction spent acid |
| CN102602904B (en) * | 2012-04-16 | 2013-09-11 | 瓮福（集团）有限责任公司 | Method for producing monoammonium phosphate from raffinate acid |
| CN102674282B (en) * | 2012-05-16 | 2014-08-20 | 瓮福（集团）有限责任公司 | Method for producing granular monoammonium phosphate |
| CN102674283A (en) * | 2012-05-20 | 2012-09-19 | 瓮福（集团）有限责任公司 | Filter residue re-slurrying method for producing crystalline monoammonium phosphate from extractive spent acid |
| CN102674284B (en) * | 2012-06-20 | 2014-06-18 | 瓮福（集团）有限责任公司 | Method for producing industrial monoammonium phosphate co-produced fertilizer grade monoammonium phosphate by extracted spent acid |
| CN102755973A (en) * | 2012-07-23 | 2012-10-31 | 瓮福（集团）有限责任公司 | Method for cleaning filtering cloth used in crystal MAP (monoammonium phosphate) production with raffinate |
| CN102786042A (en) * | 2012-08-08 | 2012-11-21 | 安徽六国化工股份有限公司 | Method for utilizing underflow sludge acid with high solid phosphorus ratio |
| CN102924158B (en) * | 2012-12-01 | 2014-03-05 | 中化化肥有限公司重庆磷复肥工程技术研究中心 | Method for producing multielement nitro-compound fertilizer |
| CN103435376A (en) * | 2013-07-29 | 2013-12-11 | 山东明瑞化工集团有限公司 | Method and apparatus used for preparing ammonium phosphate fertilizer from phosphoric acid sediment |
| CN103539170B (en) * | 2013-11-06 | 2014-12-10 | 吴杰 | Method for producing magnesium sulfate and industrial-grade monoammonium phosphate by using tail solution from refining of wet process phosphoric acid by solvent extraction method |
| CN105347321B (en) * | 2015-11-27 | 2017-08-25 | 安徽六国化工股份有限公司 | The method that phosphorus ammonium is produced using low-grade low concentration raffinate |
| CN110371939B (en) * | 2019-07-26 | 2022-08-16 | 武汉科技大学 | Preparation method of diammonium phosphate based on phosphoric acid extraction spent acid |
| CN110371944B (en) * | 2019-07-26 | 2022-08-16 | 武汉科技大学 | Method for purifying phosphoric acid raffinate acid and recovering magnesium ammonium phosphate hexahydrate |
| CN112624804A (en) * | 2020-12-24 | 2021-04-09 | 安徽六国化工股份有限公司 | Method for producing ammonium phosphate by using low-grade raffinate acid |
| CN112624074B (en) * | 2020-12-31 | 2022-11-22 | 四川龙蟒磷化工有限公司 | Method for producing industrial grade monoammonium phosphate, monopotassium phosphate and fertilizer grade monoammonium phosphate from raffinate |
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Address after: 550500 Guizhou Province, Qiannan Buyei and Miao Autonomous Prefecture Fuquan Racecourse town Yingbin Road No. 1 Wengfu group Patentee after: WENGFU GROUP Co.,Ltd. Address before: 23, 550002 floor, urn Fuk international, No. 57, South City Road, Guizhou, Guiyang Patentee before: WENGFU GROUP Co.,Ltd. |
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