CN102503591B - 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 PDFInfo
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- CN102503591B CN102503591B CN201110330494.6A CN201110330494A CN102503591B CN 102503591 B CN102503591 B CN 102503591B CN 201110330494 A CN201110330494 A CN 201110330494A CN 102503591 B CN102503591 B CN 102503591B
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- crystallizer
- phosphoric acid
- calcium nitrate
- calcium
- defluorinating agent
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process 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
Technical field
The method of a kind of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer of the present invention belongs to technical field of chemical engineering, relates to a kind of method that is applied to the preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer in the nitrocalcite crystallisation process of raw material cold method production nitrophosphate fertilizer take nitric acid and phosphorus ore.
Background technology
Be that raw material cold method is produced in the production process of nitrophosphate fertilizer with nitric acid and phosphorus ore, separated the phosphoric acid solution of acid non-soluble substance 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, the compositions such as AI, adopt the mode of indirect refrigeration crystallization will from phosphoric acid solution, isolate nitrocalcite, and the minimum temperature in nitre calcium crystallizer is controlled at-5 ℃.When hot phosphoric acid solution enters after nitre calcium crystallizer, along with the reduction of temperature, four water-calcium nitrate can be separated out from solution, the tiny crystallization that simultaneously has calcium silicofluoride, Calcium Fluoride (Fluorspan), aluminum fluosilicate, silicofluoric acid iron, magnesium silicofluoride, aluminosilicate in solution occurs, the appearance of these tiny crystalline particles not only can hinder growing up of four water-calcium nitrate crystallization, serious is, and it can stick on nitre calcium crystallizer refrigerating coil and scabs and form dirt layer, the reduction of process heat transfer coefficient, cold are increased, therefore need regularly clean refrigerating coil.Repeatedly clean the long period safe and stable operation that affects on the one hand equipment, affect on the other hand the work-ing life of equipment, in view of the singularity of nitrophosphate fertilizer system, consider from energy-conserving and environment-protective angle, adopting chemical method to carry out defluorinate processing to phosphoric acid solution ought be practicable important measures.
Summary of the invention
The object of the method for a kind of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer of the present invention is to provide a kind of method of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer; utilizing defluorinating agent to react with the fluorine in phosphoric acid solution generates precipitation defluorination and protects equipment surface; scab to solve nitre calcium crystallizer refrigerating coil, improve operation rate.
The method of a kind of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer of the present invention, it is characterized in that first the phosphoric acid solution that has separated acid non-soluble substance being carried out to defluorinate processing, under defluorinating agent normal pressure, join in the phosphoric acid solution in the nitre calcium crystallization feeding trough with whipping appts; Then between nitre calcium crystallization feeding trough and nitre calcium crystallizer, be provided with settling pocket, the precipitation forming in order to separate defluorinate process reaction; Phosphoric acid solution through defluorinate is sent in nitre calcium crystallizer.
The method of above-mentioned a kind of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer, is characterized in that the temperature of described defluorinate process phosphoric acid solution is 40-70 ℃.
The method of above-mentioned a kind of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer, it is characterized in that described defluorinating agent is the mixture of tertiary sodium phosphate and Sodium hexametaphosphate 99 or SODIUMNITRATE and Sodium hexametaphosphate 99, the weight ratio of defluorinating agent mixture is 1: 1, and defluorinating agent consumption is pressed the i.e. [Na of fluorion mole number in the sodium ion mole ratio phosphoric acid solution in defluorinating agent
+]: [F
-calculate]=1: 1.5.
The advantage of the method for a kind of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer of the present invention is: method is simple and convenient, easily implements, and processes and has effectively avoided scabbing of nitre calcium crystallizer refrigerating coil through defluorinate, has saved energy, has improved operation rate.Because the defluorinating agent adding is phosphoric acid salt and SODIUMNITRATE; with rear villiaumite precipitation and phosphoric acid and the nitric acid of generating of fluorine reaction in solution; therefore the defluorinating agent of introducing can not bring secondary pollution to system; simultaneously because the dissemination of defluorinating agent also can play protection to refrigerating coil surface; this preventing scaring to refrigerating coil has dual function, more has practical value.
Embodiment
Below in conjunction with embodiment, patent of the present invention is specifically described, but content of the present invention is not confined to the scope of cited embodiment.
First with phosphoric acid solution configuration defluorinate solution, the concentration of defluorinate solution is 6%, is dissolved in 100L phosphoric acid solution by 6g defluorinating agent.
Embodiment 1
The phosphoric acid clear liquid temperature that has separated acid non-soluble substance is 40 ℃, F
-ionic concn is 9.8g/L, and defluorinating agent is tertiary sodium phosphate and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio
+]: [F
-calculate]=1: 1.5.On nitre calcium crystallization feeding trough, be provided with defluorinate solution adding apparatus, under normal pressure, defluorinate solution joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium crystallizer, be provided with settling pocket, to separate the precipitation of defluorinate process reaction formation, send into the F of the phosphoric acid clear liquid in nitre calcium crystallizer
-ionic concn is 2.7g/L.
Embodiment 2
The phosphoric acid clear liquid temperature that has separated acid non-soluble substance is 70 ℃, F
-ionic concn is 10.5g/L, and defluorinating agent is tertiary sodium phosphate and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio
+]: [F
-calculate]=1: 1.5.On nitre calcium crystallization feeding trough, be provided with defluorinate solution adding apparatus, under normal pressure, defluorinate solution joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium crystallizer, be provided with settling pocket, to separate the precipitation of defluorinate process reaction formation, send into the F of the phosphoric acid clear liquid in nitre calcium crystallizer
-ionic concn is 4.3g/L.
Embodiment 3
The phosphoric acid clear liquid temperature that has separated acid non-soluble substance is 50 ℃, F
-ionic concn is 8.9g/L, and defluorinating agent is tertiary sodium phosphate and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio
+]: [F
-calculate]=1: 1.5.On nitre calcium crystallization feeding trough, be provided with defluorinate solution adding apparatus, under normal pressure, defluorinate solution joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium crystallizer, be provided with settling pocket, to separate the precipitation of defluorinate process reaction formation, send into the F of the phosphoric acid clear liquid in nitre calcium crystallizer
-ionic concn is 3.1g/L.
Embodiment 4
The phosphoric acid clear liquid temperature that has separated acid non-soluble substance is 50 ℃, F
-ionic concn is 11.0g/L, and defluorinating agent is tertiary sodium phosphate and Sodium hexametaphosphate 99, and consumption is [Na in molar ratio
+]: [F
-calculate]=1: 1.5.On nitre calcium crystallization feeding trough, be provided with defluorinate solution adding apparatus, under normal pressure, defluorinate solution joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium crystallizer, be provided with settling pocket, to separate the precipitation of defluorinate process reaction formation, send into the F of the phosphoric acid clear liquid in nitre calcium crystallizer
-ionic concn is 3.9g/L.
Embodiment 5
The phosphoric acid clear liquid temperature that has 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.On nitre calcium crystallization feeding trough, be provided with defluorinate solution adding apparatus, under normal pressure, defluorinate solution joined in the phosphoric acid clear liquid in the nitre calcium crystallization feeding trough with whipping appts.Between nitre calcium crystallization feeding trough and nitre calcium crystallizer, be provided with settling pocket, to separate the precipitation of defluorinate process reaction formation, send into the F of the phosphoric acid clear liquid in nitre calcium crystallizer
-ionic concn is 4.0g/L.
Claims (2)
1. a method for preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer, is characterized in that first the phosphoric acid solution that has separated acid non-soluble substance being carried out to defluorinate processing, joins in the phosphoric acid solution in the nitre calcium crystallization feeding trough with whipping appts under defluorinating agent normal pressure; Then between nitre calcium crystallization feeding trough and nitre calcium crystallizer, be provided with settling pocket, the precipitation forming in order to separate defluorinate process reaction; Phosphoric acid solution through defluorinate is sent in nitre calcium crystallizer; Described defluorinating agent is the mixture of tertiary sodium phosphate and Sodium hexametaphosphate 99 or SODIUMNITRATE and Sodium hexametaphosphate 99, and the weight ratio of defluorinating agent mixture is 1:1, and defluorinating agent consumption is pressed the i.e. [Na of fluorion mole number in the sodium ion mole ratio phosphoric acid solution in defluorinating agent
+]: [F
-]=1:1.5 calculates.
2. according to the method for a kind of preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer claimed in claim 1, it is characterized in that the temperature of described defluorinate process phosphoric acid solution is 40-70 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110330494.6A CN102503591B (en) | 2011-10-20 | 2011-10-20 | Method for preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer |
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|---|---|---|---|
| CN201110330494.6A CN102503591B (en) | 2011-10-20 | 2011-10-20 | Method for preventing scars of refrigerating coil of calcium nitrate crystallizer for nitrophosphate fertilizer |
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| Publication Number | Publication Date |
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| CN102503591A CN102503591A (en) | 2012-06-20 |
| CN102503591B true CN102503591B (en) | 2014-05-14 |
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| CN103073344B (en) * | 2013-01-23 | 2014-10-15 | 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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|---|---|---|---|---|
| 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 |
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