CN104072209A - Method for preparing nitro compound fertilizer by adopting acid sludge produced in the phosphoric acid manufacturing process - Google Patents

Method for preparing nitro compound fertilizer by adopting acid sludge produced in the phosphoric acid manufacturing process Download PDF

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Publication number
CN104072209A
CN104072209A CN201410338769.4A CN201410338769A CN104072209A CN 104072209 A CN104072209 A CN 104072209A CN 201410338769 A CN201410338769 A CN 201410338769A CN 104072209 A CN104072209 A CN 104072209A
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China
Prior art keywords
acid
phosphoric acid
compound fertilizer
sludge
acid sludge
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CN201410338769.4A
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Chinese (zh)
Inventor
陈爱中
刘兵
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YUNNAN CHANGQINGSHU CHEMICALS CO Ltd
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YUNNAN CHANGQINGSHU CHEMICALS CO Ltd
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Priority to CN201410338769.4A priority Critical patent/CN104072209A/en
Publication of CN104072209A publication Critical patent/CN104072209A/en
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Abstract

The invention provides a method for preparing nitro compound fertilizer by adopting acid sludge produced in the phosphoric acid manufacturing process. The nitro compound fertilizer is prepared by adopting phosphoric acid sludge produced in the phosphoric acid manufacturing process as the raw material, and adding nitric acid and ammonia for reaction. The method comprises the following steps: (1) centrifugally separating the phosphoric acid sludge produced in the phosphoric acid manufacturing process, totally recycling the phosphoric acid, and taking the sludge as the manufacturing raw material of the nitro compound fertilizer; (2) preparing a solution on the basis of a proportion of 55-60% of dry contents after centrifugal separation of the acid sludge, stirring and adding 40% of nitric acid according to the mass ratio at the room temperature for reaction; (3) in the reaction process, pumping in ammonia for acid-alkali neutralization, and controlling the PH value of the slurry to be 5.5-5.7; (4) after reaction, performing spraying granulation, drying, sieving, smashing, finished product cooling and packaging on the slurry by a granulator. The method is simple in process, convenient to operate, capable of reacting at the room temperature, free of external heat quantity and low in energy consumption; by the adoption of the acid sludge as the raw material, the phosphorus resource is maximally utilized, and products containing nitrate nitrogen can be absorbed by plants easily.

Description

A kind ofly utilize the acid sludge in phosphoric acid production to prepare nitro-compound fertilizer method
Technical field
The invention belongs to the method and technology field that utilizes the acid sludge producing in production process of phosphoric acid to prepare nitro-compound fertilizer.
Technical background
Acid sludge is the impurity being brought by phosphorus ore in production process of phosphoric acid, is mainly the salt that the zwitterion such as Fe, Al, Ca, Mg, K, Na, F, S forms, at Phosphoric Acid Concentration process and phosphoric acid storage process along with a large amount of precipitations are separated out in the decline of temperature.These precipitations are by being exactly acid sludge after centrifugation.These deposited salts and postprecipitation salt are substantially water insoluble, belong to insoluble phosphorus.
Nitro-compound fertilizer is to take ammonium nitrate as nitrogenous source, adds the compound fertilizer raw materials such as phosphorus, potassium, the N producing, P, K high-concentration compound fertilizer material.In its product, not only contain nitric nitrogen but also contain ammonia-state nitrogen.Main products has ammonium nitrate phosphorus, ammonium nitrate phosphorus potassium.
Acid sludge, as producing ammonium nitrate phosphorus nitro-compound fertilizer raw material, is different from other and adds the former element compound (mixed) fertilizer raw material of phosphorus.Seek a kind of acid sludge and process more scientific, reasonable, feasible method.
The treatment process of acid sludge is subject to the foreign matter content of acid sludge own high, and poorly water-soluble, the impact that free acid is high, be directly used in agriculture production as a kind of chemical fertilizer, is subject to water-soluble not high impact, and plant is difficult to absorb effective constituent; Be subject to the higher impact of free acid, plant cannot survive under the high condition of acidic conditions.Acid sludge after must processing by other method could be used for agricultural fertilizer.Existing treatment method of acid residuum has following several:
1, acid sludge, not by centrifugation, utilizes the phosphoric acid direct production agricultural level monoammonium phosphate of certain solid content.As existing slurry concentration process monoammonium phosphate, Traditional Method monoammonium phosphate, high tower spraying powdery monoammonium phosphate etc.
2, acid sludge by centrifugation after supplementing for general calcium production process phosphorus.
3, acid sludge by centrifugation after supplementing for rich calcium production process phosphorus.
4, composite fertilizer produces for phosphoric raw material.
Along with the raising of existing phosphate fertilizer technological standard, for general calcium, rich calcium, composite fertilizer, there is the requirement to water-soluble phosphorus content.Acid sludge, with for the extremely low raw material of a kind of water-soluble phosphorus content is used, is subject to very large restriction in utilization ratio.
Along with sulphur dioxide of phosphor chemical industry product up-gradation, a large amount of PHOSPHORIC ACID TECH.GRADE product salts arise.Phosphoric acid is as the raw material of PHOSPHORIC ACID TECH.GRADE product salt, just higher to the specification of quality of phosphoric acid.Will certainly produce more acid sludge.Therefore the disposal and utilization of acid sludge will be a new research topic and direction.
General calcium product operative norm: GB20413-2006 (although this standard is not stipulated the requirement of water-soluble phosphorus, country modifies to this standard now, brings water-soluble phosphorus content into standard)
Rich calcium product operative norm: DB53/523-2013
Coarse whiting product operative norm: GB21634-2008
Summary of the invention
Object of the present invention provides a kind of in order to overcome defect that above-mentioned prior art exists and weak point just and utilizes the acid sludge in phosphoric acid production to prepare nitro-compound fertilizer method.
The object of the invention is to realize by following technical solution.
Utilize the acid sludge in phosphoric acid production to prepare a nitro-compound fertilizer method, the present invention is characterised in that: adopting the phosphoric acid slag producing in production process of phosphoric acid is raw material, adds nitric acid, gas ammonia to react and obtains nitro-compound fertilizer; Comprise the following steps:
, the phosphoric acid slag that produces of production process of phosphoric acid is through centrifugation, and phosphoric acid is all reclaimed, acid sludge is made nitro-compound fertilizer raw materials for production;
(2) the acid sludge, after centrifugation is mixed with solution according to the ratio of 55%-60% solid content, adds 40% nitric acid stirring, under normal temperature according to mass ratio, reacts;
, pass into gas ammonia in reaction process and carry out acid-base neutralisation, controlling slip pH value is 5.5-5.7;
(4), reacted slip through tablets press spray granulating, dry, screening, broken, finished product is cooling, packing.
The index request of described acid sludge is:
Available phosphorus % Water-soluble phosphorus % Free acid % Water-soluble phosphorus/available phosphorus % Moisture %
40-42 9.5-11.5 10-12 20-30 6.5-8.5
Friendship effect of the present invention: this method technique is simple, easy to operate, reaction is reaction at normal temperatures, without outer increase heat, less energy-consumption; And use acid sludge is raw material, the maximum using of phosphor resource contains nitric nitrogen in product.More easily by plant, absorbed.
Accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
Embodiment mono-
, the phosphoric acid slag that produces of production process of phosphoric acid is through centrifugation, and phosphoric acid is all reclaimed, acid sludge is made nitro-compound fertilizer raw materials for production;
Acid sludge index:
Available phosphorus % Water-soluble phosphorus % Free acid % Water-soluble phosphorus/available phosphorus % Moisture %
41 10.2 11.2 24.88 7.24
(2) the acid sludge, after centrifugation is mixed with solution according to the ratio of 55% solid content, adds the nitric acid of 40% concentration stirring, under normal temperature according to mass ratio, reacts;
, pass into gas ammonia in reaction process and carry out acid-base neutralisation, controlling slip pH value is 5.7;
(4), reacted slip through tablets press spray granulating, dry, screening, broken, finished product is cooling, packing.
Embodiment bis-
, the phosphoric acid slag that produces of production process of phosphoric acid is through centrifugation, and phosphoric acid is all reclaimed, acid sludge is made nitro-compound fertilizer raw materials for production;
Acid sludge index:
Available phosphorus % Water-soluble phosphorus % Free acid % Water-soluble phosphorus/available phosphorus % Moisture %
40.2 9.8 11.3 24.38 8.03
(2) the acid sludge, after centrifugation is mixed with solution according to the ratio of 60% solid content, adds the nitric acid of 40% concentration stirring, under normal temperature according to mass ratio, reacts;
, pass into gas ammonia in reaction process and carry out acid-base neutralisation, controlling slip pH value is 5.5;
(4), reacted slip through tablets press spray granulating, dry, screening, broken, finished product is cooling, packing.

Claims (2)

1. utilize the acid sludge in phosphoric acid production to prepare a nitro-compound fertilizer method, it is characterized in that, adopting the phosphoric acid slag producing in production process of phosphoric acid is raw material, adds nitric acid, gas ammonia to react and obtains nitro-compound fertilizer; Comprise the following steps:
, the phosphoric acid slag that produces of production process of phosphoric acid is through centrifugation, and phosphoric acid is all reclaimed, acid sludge is made nitro-compound fertilizer raw materials for production;
(2) the acid sludge, after centrifugation is mixed with solution according to the ratio of 55%-60% solid content, adds 40% nitric acid stirring, under normal temperature according to mass ratio, reacts;
, pass into gas ammonia in reaction process and carry out acid-base neutralisation, controlling slip pH value is 5.5-5.7;
(4), reacted slip through tablets press spray granulating, dry, screening, broken, finished product is cooling, packing.
2. as claimed in claim 1ly a kind ofly utilize the acid sludge in phosphoric acid production to prepare nitro-compound fertilizer method, it is characterized in that, the index request of described acid sludge is:
Available phosphorus % Water-soluble phosphorus % Free acid % Water-soluble phosphorus/available phosphorus % Moisture % 40-42 9.5-11.5 10-12 20-30 6.5-8.5
CN201410338769.4A 2014-07-16 2014-07-16 Method for preparing nitro compound fertilizer by adopting acid sludge produced in the phosphoric acid manufacturing process Pending CN104072209A (en)

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CN201410338769.4A CN104072209A (en) 2014-07-16 2014-07-16 Method for preparing nitro compound fertilizer by adopting acid sludge produced in the phosphoric acid manufacturing process

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CN201410338769.4A CN104072209A (en) 2014-07-16 2014-07-16 Method for preparing nitro compound fertilizer by adopting acid sludge produced in the phosphoric acid manufacturing process

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106278390A (en) * 2016-07-19 2017-01-04 中化化肥有限公司成都研发中心 A kind of phosphoric acid by wet process acid sludge comprehensive reutilization method
CN107879849A (en) * 2017-11-27 2018-04-06 潘桂花 The agricultural organic composite fertilizer slurry-spraying pelletizing technique of green
CN107954546A (en) * 2017-11-24 2018-04-24 天峨县平昌生态农业有限公司 A kind of processing method for cultivating family's poultry waster water

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102040206A (en) * 2010-11-02 2011-05-04 昆明川金诺化工有限公司 Method for recycling acid sludge produced by concentrated phosphoric acid
CN102173904A (en) * 2011-01-20 2011-09-07 山东金正大生态工程股份有限公司 Method for producing compound mixed fertilizer by utilizing solid isolate from phosphorite decomposed with nitric acid
CN102924158A (en) * 2012-12-01 2013-02-13 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
CN103113139A (en) * 2013-03-05 2013-05-22 中化化肥有限公司重庆磷复肥工程技术研究中心 Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102040206A (en) * 2010-11-02 2011-05-04 昆明川金诺化工有限公司 Method for recycling acid sludge produced by concentrated phosphoric acid
CN102173904A (en) * 2011-01-20 2011-09-07 山东金正大生态工程股份有限公司 Method for producing compound mixed fertilizer by utilizing solid isolate from phosphorite decomposed with nitric acid
CN102924158A (en) * 2012-12-01 2013-02-13 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
CN103113139A (en) * 2013-03-05 2013-05-22 中化化肥有限公司重庆磷复肥工程技术研究中心 Method for producing multivariate nitro compound fertilizer from wet-process phosphoric acid purification sludge
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

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106278390A (en) * 2016-07-19 2017-01-04 中化化肥有限公司成都研发中心 A kind of phosphoric acid by wet process acid sludge comprehensive reutilization method
CN107954546A (en) * 2017-11-24 2018-04-24 天峨县平昌生态农业有限公司 A kind of processing method for cultivating family's poultry waster water
CN107879849A (en) * 2017-11-27 2018-04-06 潘桂花 The agricultural organic composite fertilizer slurry-spraying pelletizing technique of green

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Application publication date: 20141001