CN102503591A - Method for preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer - Google Patents

Method for preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer Download PDF

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Publication number
CN102503591A
CN102503591A CN2011103304946A CN201110330494A CN102503591A CN 102503591 A CN102503591 A CN 102503591A CN 2011103304946 A CN2011103304946 A CN 2011103304946A CN 201110330494 A CN201110330494 A CN 201110330494A CN 102503591 A CN102503591 A CN 102503591A
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phosphoric acid
calcium
nitre
mold
calcium nitrate
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CN2011103304946A
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CN102503591B (en
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樊彩梅
李双志
荆宏健
冯军强
魏安根
王志华
刘金亮
张凌云
李�瑞
高海生
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Taiyuan University of Technology
Tianji Coal Chemical Industry Group Co Ltd
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Taiyuan University of Technology
Tianji Coal Chemical Industry Group Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

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Abstract

The invention discloses a method for preventing scars of a refrigerating coil of a calcium nitrate crystallizer for a nitrophosphate fertilizer, and belongs to the technical field of chemical engineering. According to the method, a clear liquid of phosphoric acid with acid-insoluble substances being separated is subjected to defluorination, a defluorinating agent is added into a calcium nitrate crystallization feed tank with a stirrer device under normal pressure, a settling chamber is formed between the calcium nitrate crystallization feed tank and the calcium nitrate crystallizer to separate precipitates formed in reaction of the defluorination process, and the defluorinated clear liquid of phosphoric acid enters the calcium nitrate crystallizer. The method is simple and convenient, and is easy to implement; through defluorination, the scars of the refrigerating coil of the calcium nitrate crystallizer are effectively avoided, energy is saved, and the operation rate is improved; and the introduced defluorinating agent cannot bring secondary pollution to the system.

Description

A kind of method of nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring
Technical field
The method of a kind of nitrophosphate fertilizer nitre of the present invention calcium mold refrigerating coil preventing scaring belongs to technical field of chemical engineering, relates to that a kind of to be applied to nitric acid and phosphorus ore be the method that the raw material cold method is produced the nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring in the nitrocalcite crystallisation process of nitrophosphate fertilizer.
Background technology
Use nitric acid and phosphorus ore to produce in the production process of nitrophosphate fertilizer as the raw material cold method, the phosphoric acid solution that has separated acid non-soluble substance is by H 3PO 4, HNO 3, H 2SiF 4, HF, Ca (NO 3) 2, Al (NO 3) 3, Fe (NO 3) 2, Mg (NO 3) 2, compositions such as AI adopt indirect refrigeration crystalline mode will from phosphoric acid solution, isolate nitrocalcite, and the minimum temperature in the nitre calcium mold is controlled at-5 ℃.After hot phosphoric acid solution gets into nitre calcium mold; Reduction along with temperature; Four water-calcium nitrate can be separated out from solution; The tiny crystallization that has calcium silicofluoride, Calcium Fluoride (Fluorspan), aluminum fluosilicate, silicofluoric acid iron, magnesium silicofluoride, aluminosilicate simultaneously in the solution occurs, and the appearance of these tiny crystalline particles not only can hinder the four water-calcium nitrate crystalline to grow up, and serious is that it can stick to the formation dirt layer that scabs on the nitre calcium mold refrigerating coil; The reduction of process heat transfer coefficient, cold are increased, so need regularly clean to refrigerating coil.Clean the LP safe and stable operation that influences equipment on the one hand repeatedly; Influence the work-ing life of equipment on the other hand; In view of the singularity of nitrophosphate fertilizer system, consider that from the energy-conserving and environment-protective angle method that adopts chemistry is carried out defluorinate to phosphoric acid solution and handled when being practicable important measures.
Summary of the invention
The purpose of the method for a kind of nitrophosphate fertilizer nitre of the present invention calcium mold refrigerating coil preventing scaring is to provide a kind of method of nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring; Utilize the fluorine reaction in defluorinating agent and the phosphoric acid solution to generate the deposition defluorination and protect equipment surface; Scab to solve nitre calcium mold refrigerating coil, improve operation rate.
The method of a kind of nitrophosphate fertilizer nitre of the present invention calcium mold refrigerating coil preventing scaring; It is characterized in that at first the phosphoric acid solution that has separated acid non-soluble substance being carried out defluorinate handles, and joins under the defluorinating agent normal pressure in the phosphoric acid solution in the nitre calcium crystallization feeding trough of being with whipping appts; Between nitre calcium crystallization feeding trough and nitre calcium mold, be provided with settling pocket then, in order to separate the deposition that the defluorinate process reaction forms; Phosphoric acid solution through defluorinate is sent in the nitre calcium mold.
The method of above-mentioned a kind of nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring, the temperature that it is characterized in that described defluorinate process phosphoric acid solution is 40-70 ℃.
The method of above-mentioned a kind of nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring; It is characterized in that described defluorinating agent is the mixture of tsp and Sodium hexametaphosphate 99 or SODIUMNITRATE and Sodium hexametaphosphate 99; The weight ratio of defluorinating agent mixture is 1: 1, and the fluorion mole number that the defluorinating agent consumption is pressed in the sodium ion mole ratio phosphoric acid solution in the defluorinating agent is [Na +]: [F -Calculate]=1: 1.5.
The advantage of the method for a kind of nitrophosphate fertilizer nitre of the present invention calcium mold refrigerating coil preventing scaring is: method is simple and convenient, implements easily, handles through defluorinate and has effectively avoided scabbing of nitre calcium mold refrigerating coil, has practiced thrift energy, has improved operation rate.Because the defluorinating agent that adds is phosphoric acid salt and SODIUMNITRATE; Generate villiaumite deposition and phosphoric acid and nitric acid with the fluorine reaction back in the solution; Therefore the defluorinating agent of introducing can not bring secondary pollution to system; Because the dissemination of defluorinating agent also can play protection to the refrigerating coil surface, this preventing scaring to refrigerating coil has dual function, has more practical value simultaneously.
Embodiment
To combine embodiment that patent of the present invention is specifically explained below, but content of the present invention is not confined to the scope of cited embodiment.
At first with phosphoric acid solution configuration defluorinate solution, the concentration of defluorinate solution is 6%, is about to the 6g defluorinating agent and is dissolved in the 100L phosphoric acid solution.
Embodiment 1
The phosphoric acid clear liquid temperature of having separated acid non-soluble substance is 40 ℃, F -Ionic concn is 9.8g/L, and defluorinating agent is tsp and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio +]: [F -Calculate]=1: 1.5.Nitre calcium crystallization feeding trough is provided with defluorinate solution adding apparatus, under the normal pressure defluorinate solution is joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough of being with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium mold, be provided with settling pocket,, send into the F of the phosphoric acid clear liquid in the nitre calcium mold to separate the deposition that the defluorinate process reaction forms -Ionic concn is 2.7g/L.
Embodiment 2
The phosphoric acid clear liquid temperature of having separated acid non-soluble substance is 70 ℃, F -Ionic concn is 10.5g/L, and defluorinating agent is tsp and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio +]: [F -Calculate]=1: 1.5.Nitre calcium crystallization feeding trough is provided with defluorinate solution adding apparatus, under the normal pressure defluorinate solution is joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough of being with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium mold, be provided with settling pocket,, send into the F of the phosphoric acid clear liquid in the nitre calcium mold to separate the deposition that the defluorinate process reaction forms -Ionic concn is 4.3g/L.
Embodiment 3
The phosphoric acid clear liquid temperature of having separated acid non-soluble substance is 50 ℃, F -Ionic concn is 8.9g/L, and defluorinating agent is tsp and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio +]: [F -Calculate]=1: 1.5.Nitre calcium crystallization feeding trough is provided with defluorinate solution adding apparatus, under the normal pressure defluorinate solution is joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough of being with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium mold, be provided with settling pocket,, send into the F of the phosphoric acid clear liquid in the nitre calcium mold to separate the deposition that the defluorinate process reaction forms -Ionic concn is 3.1g/L.
Embodiment 4
The phosphoric acid clear liquid temperature of having separated acid non-soluble substance is 50 ℃, F -Ionic concn is 11.0g/L, and defluorinating agent is tsp and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio +]: [F -Calculate]=1: 1.5.Nitre calcium crystallization feeding trough is provided with defluorinate solution adding apparatus, under the normal pressure defluorinate solution is joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough of being with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium mold, be provided with settling pocket,, send into the F of the phosphoric acid clear liquid in the nitre calcium mold to separate the deposition that the defluorinate process reaction forms -Ionic concn is 3.9g/L.
Embodiment 5
The phosphoric acid clear liquid temperature of having separated acid non-soluble substance is 60 ℃, F -Ionic concn is 9.8g/L, and defluorinating agent is SODIUMNITRATE and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio +]: [F -Calculate]=1: 1.5.Nitre calcium crystallization feeding trough is provided with defluorinate solution adding apparatus, under the normal pressure defluorinate solution is joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough of being with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium mold, be provided with settling pocket,, send into the F of the phosphoric acid clear liquid in the nitre calcium mold to separate the deposition that the defluorinate process reaction forms -Ionic concn is 4.0g/L.

Claims (3)

1. the method for a nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring is characterized in that at first the phosphoric acid solution that has separated acid non-soluble substance being carried out defluorinate handles, and joins under the defluorinating agent normal pressure in the phosphoric acid solution in the nitre calcium crystallization feeding trough of being with whipping appts; Between nitre calcium crystallization feeding trough and nitre calcium mold, be provided with settling pocket then, in order to separate the deposition that the defluorinate process reaction forms; Phosphoric acid solution through defluorinate is sent in the nitre calcium mold.
2. according to the method for the described a kind of nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring of claim 1, the temperature that it is characterized in that described defluorinate process phosphoric acid solution is 40-70 ℃.
3. according to the method for the described a kind of nitrophosphate fertilizer nitre calcium mold refrigerating coil preventing scaring of claim 1; It is characterized in that described defluorinating agent is the mixture of tsp and Sodium hexametaphosphate 99 or SODIUMNITRATE and Sodium hexametaphosphate 99; The weight ratio of defluorinating agent mixture is 1: 1, and the fluorion mole number that the defluorinating agent consumption is pressed in the sodium ion mole ratio phosphoric acid solution in the defluorinating agent is [Na +]: [F -Calculate]=1: 1.5.
CN201110330494.6A 2011-10-20 2011-10-20 Method for preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer Active CN102503591B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103073344A (en) * 2013-01-23 2013-05-01 天脊煤化工集团股份有限公司 Production method for high-concentration defluorinate nitronitrogen phosphorus and potassium compound fertilizer

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02267178A (en) * 1989-04-05 1990-10-31 Minamikiyuushiyuu Kagaku Kogyo Kk Fused phosphate fertilizer and preparation thereof
HU214285B (en) * 1993-09-08 1998-03-02 Remi and Mediterrán Kft. Continuous or step-by-step method for production of fertilizer or feed quality phosphates
CN101708832A (en) * 2009-11-02 2010-05-19 山东红日阿康化工股份有限公司 Method for producing defluorinated ammonium phosphate
CN101786741A (en) * 2010-02-21 2010-07-28 瓮福(集团)有限责任公司 Method for defluorinating acid waste water with high fluorine

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02267178A (en) * 1989-04-05 1990-10-31 Minamikiyuushiyuu Kagaku Kogyo Kk Fused phosphate fertilizer and preparation thereof
HU214285B (en) * 1993-09-08 1998-03-02 Remi and Mediterrán Kft. Continuous or step-by-step method for production of fertilizer or feed quality phosphates
CN101708832A (en) * 2009-11-02 2010-05-19 山东红日阿康化工股份有限公司 Method for producing defluorinated ammonium phosphate
CN101786741A (en) * 2010-02-21 2010-07-28 瓮福(集团)有限责任公司 Method for defluorinating acid waste water with high fluorine

Non-Patent Citations (1)

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Title
杨林军,等: "湿法磷酸过滤系统结垢特性及防治研究进展", 《化肥工业》, vol. 28, no. 5, 31 October 2001 (2001-10-31) *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103073344A (en) * 2013-01-23 2013-05-01 天脊煤化工集团股份有限公司 Production method for high-concentration defluorinate nitronitrogen phosphorus and potassium compound fertilizer

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