CN103073344A - Production method for high-concentration defluorinate nitronitrogen phosphorus and potassium compound fertilizer - Google Patents

Production method for high-concentration defluorinate nitronitrogen phosphorus and potassium compound fertilizer Download PDF

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CN103073344A
CN103073344A CN2013100241906A CN201310024190A CN103073344A CN 103073344 A CN103073344 A CN 103073344A CN 2013100241906 A CN2013100241906 A CN 2013100241906A CN 201310024190 A CN201310024190 A CN 201310024190A CN 103073344 A CN103073344 A CN 103073344A
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mother liquor
acid
defluorinate
compound fertilizer
potassium
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CN103073344B (en
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荆宏健
樊彩梅
冯军强
畅学华
王志华
魏安根
刘金亮
李�瑞
高海生
李双志
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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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Abstract

The invention discloses a production method for high-concentration defluorinate nitro nitrogen phosphorus and potassium compound fertilizer, which is based on the conventional process route of nitric acid phosphatic manure production, an acid-insoluble substance deep desorbing procedure is added in an acid-insoluble substance precipitation separation procedure so as to radically separate the acid-insoluble substance; a mother liquor defluorinating procedure is added between calcium nitrate filtration and mother liquor neutralization, by adding potassium nitrate into mother liquor, fluosilicic acid ions in mother liquor is reacted with potassium ion to generate potassium fluorosilicate product, after defluorinating reaction, potassium fluorosilicate is separated from slurry through filtering and separating, and ammonia neutralization, evaporation, pelletization, drying and cooling treatment are performed on defluorinated mother liquor by adding potassium nitrate and ammonium nitrate, namely, high-concentration nitro nitrogen phosphorus and potassium compound fertilizer is obtained. In the invention, mid low grade phosphate rock is used for preparing compound fertilizer, namely fluorine resource is recycled, and by-product potassium fluorosilicate is obtained, pollutions to the environment are reduced, the obtained product has an excellent performance, chlorine is not contained, the application range is broad, the probability of caking is low, and the market competitiveness is strong.

Description

A kind of production method of defluorinate high density nitro azophoska compound fertilizer
Technical field
The invention belongs to chemical production technical field, be specifically related to a kind of production method of defluorinate high density nitro azophoska compound fertilizer.
Background technology
At present, nitro-compound fertilizer on the market generally is take ammonium nitrate as nitrogenous source, by adding the multiple fertile raw material such as phosphorus, potassium, the N that produces, P, K high-concentration compound fertilizer material.With decomposing phosphorite by using nitric acid, cold method deliming explained hereafter nitro phosphor complex, operational path is advanced, and fertilizer variety is good, and agricultural effect is obvious, plays an important role in national economy.
From current fertilizer selling price situation, the price of nitrophosphate fertilizer unit nutrient is minimum in various composite fertilizers, has very strong competitive edge, in the production of Nitro Phosphate Unit basis exploitation nitro multi-component composite fertilizer, is necessary and with the obvious advantage.But the situation that faces at present is that phosphate rock resource is in short supply, grade constantly descends, Chinese P 2O 5〉=30% abundant ore source only can use 2014 (Zhang Weifeng, Marvin's is strange, Zhang Fusuo etc., natural resources journal, 2005,20 (3): 378-386; Lu Rukun, soil, 2004,36 (1): 1-4).Along with the continuous minimizing of high-quality phosphorus ore reserves, no matter be domestic or external, the multiple fertile enterprise of phosphorus all will be faced with the predicament of using low-grade phosphate ore to produce, particularly be engaged in the enterprise that high concentration nitric-phosphate fertilizer is produced.On the other hand, along with improving constantly of the whole knowledge in rural area, scientific and technological level, the composite fertilizer of multiple nutrient structure and soil testing and fertilizer recommendation more and more are subjected to friend's peasant concern, providing comprehensive, collaborative N, P, the K composite fertilizer that absorbs of crop nutrition content to become the inexorable trend of modern chemical fertilizer development, also is one of responsibility of fertilizer enterprises.And along with the raising of environmental requirement and people's consciousness, the pollution problem of bringing fluorine in the fertilizer system with phosphorus ore into needs to solve.
The technical process of Phosphate Fertilizer Nitrate with Frozen Method be phosphorus ore add that nitric acid carries out that acid non-soluble substance precipitate and separate, nitrocalcite freezing and crystallizing from acid hydrolysis solution in acidolysis, the acid hydrolysis solution separated out, nitrocalcite filters, the mother liquor that filters to isolate from nitrocalcite carries out the ammonia neutralization, and the slip evaporation, then granulation, drying, cooling namely get the nitrophosphate fertilizer product, wherein the fluorochemical in the phosphorus ore 80% is transferred in the mother liquor, finally enters the nitrophosphate fertilizer product.Nitrophosphate fertilizer product total nutrient wherein contains P greater than 38% 2O 5~ 12.5%, N ~ 25%, other nutrients ~ 2%.The original design raw material phosphorus ore grade that requires of this technique is higher, and the phosphorus ore quality index must satisfy P 2O 5〉=31%, MgO≤1.0%, AI≤10%.But reality is that grade and the quality of phosphorus ore descending year by year, and enterprise must be faced with the use mid low grade phosphate rock.If produce with the mid low grade phosphate rock tissue, must be on the existing apparatus basis, the development of new operational path is eliminated the fluoride pollution problem, could solve low-grade phosphate ore and produce the technical barrier of high concentration nitric-phosphate fertilizer, nitro azophoska compound fertilizer, also could adapt to the market structure of China's phosphate rock resource.
China's chemical fertilizer nutrient structure is take nitrogen as main, and it is also more serious to lack the few potassium phenomenon of phosphorus, and according to detection, the average demand of N, P, K is with N:P in China's fertilizer 2O 5: K 2O=1:0.6:0.35 (Chinese patent CN1182085C) is best, and in fact the growth demand of crop is still take nitrogenous fertilizer as main.N:P in the nitrophosphate fertilizer product 2O 5Ratio is 1:0.5, near the best N∶P ratio of demand, by add all good saltpetre of consistency, suitability to system, eliminates fluoride pollution when realizing nitro azophoska compound fertilizer production and reclaims the fluorine resource.Therefore, the Technology at existing Nitro Phosphate Unit basis development and use mid low grade phosphate rock stone production high density defluorinate nitro azophoska compound fertilizer has strategic importance.
Summary of the invention
The object of the invention is intended to overcome the deficiency of existing production high density nitro azophoska compound fertilizer processing method, provide a kind of technique simple, reduce pollute, with the production method of mid low grade phosphate rock production defluorinate high density nitro azophoska compound fertilizer, namely produce total nutrient greater than the production method of 40% nitro azophoska compound fertilizer with mid low grade phosphate rock.
For achieving the above object, the present invention adopts following solution: a kind of production method of defluorinate high density nitro azophoska compound fertilizer, be based on the existing operational path of producing nitrophosphate fertilizer, comprise following step successively: phosphorus ore adds nitric acid solution, acid non-soluble substance precipitate and separate, nitrocalcite freezing and crystallizing, nitrocalcite filtration, mother liquor neutralization, evaporation, granulation and drying, it is characterized in that: increased acid non-soluble substance deep removal process in acid non-soluble substance precipitate and separate step, between nitrocalcite filtration and two steps of mother liquor neutralization, increased mother liquor defluorinate step.
The production method of above-mentioned a kind of defluorinate high density nitro azophoska compound fertilizer is characterized in that: described acid non-soluble substance deep removal process is:
1) precipitate and separate process: acid hydrolysis solution is precipitated, filters, make the acid non-soluble substance in the acid hydrolysis solution carry out preliminary separation;
2) acid non-soluble substance deep removal process: to initial gross separation the acid hydrolysis solution of acid non-soluble substance add flocculation agent, then flocculation sediment 0.5-1 hour carries out filtration treatment, the acid hydrolysis solution that has removed acid non-soluble substance is sent to the nitrocalcite freezing and crystallizing.
The production method of above-mentioned a kind of defluorinate high density nitro azophoska compound fertilizer is characterized in that: described mother liquor defluorinate step comprises following process:
1) defluorinate process: add saltpetre to mother liquor, make silicofluoric acid ion and potassium ion reaction in the mother liquor generate the potassium silicofluoride crystallization, the process reaction condition is 10-50 ℃ of temperature of reaction, 0.5-1 hour reaction times, the add-on of saltpetre is pressed the silicofluoric acid content in the mother liquor and is decided, and namely the mol ratio of saltpetre and silicofluoric acid is: 2-4;
2) solid-liquid separation process: the slip behind the defluorination reaction is separated by filtration out the solid phase prod potassium silicofluoride, and filtrate is the defluorinate mother liquor, is sent in next step and operation.
The production method of above-mentioned a kind of defluorinate high density nitro azophoska compound fertilizer, it is characterized in that: according to the requirement of fertilizer product to N-P-K content, add saltpetre and ammonium nitrate to adjust the nitrogen phosphoris and potassium fertilizer ratio of fertilizer product at the mother liquor N-process, the addition of saltpetre is 0.2-0.4 with the phosphorus ore quality ratio, and the addition of ammonium nitrate is 0.12-0.20 with the phosphorus ore quality ratio.
The production method of above-mentioned a kind of defluorinate high density nitro azophoska compound fertilizer is characterized in that: in order to adjust the potassium content in the fertilizer product, the saltpetre that adds also can add at granulation process.
The production method of above-mentioned a kind of defluorinate high density nitro azophoska compound fertilizer is characterized in that: add in the nitric acid solution process at phosphorus ore, described phosphorus ore is mid low grade phosphate rock, wherein P 2O 521%-30wt%, MgO≤2.0wt%, Fe 2(Al 2O) 3≤ 3.5wt %, F≤3.0wt%, AI≤20wt%.
Design of the present invention mainly is on Phosphate Fertilizer Nitrate with Frozen Method technical process basis, namely add on the basis of the operations such as nitric acid solution, acid non-soluble substance precipitate and separate, nitrocalcite freezing and crystallizing, nitrocalcite filtration, mother liquor neutralization, evaporation, granulation, drying, cooling at phosphorus ore, increased acid non-soluble substance deep removal process in acid non-soluble substance precipitate and separate step, by adding flocculation agent to acid hydrolysis solution acid non-soluble substance has further been removed; For the fluoride pollution of eliminating in the fertilizer reclaims the fluorine resource, between nitrocalcite filtration and two steps of mother liquor neutralization, increased mother liquor defluorinate step, according to the method for the generation of the silicofluoric acid in saltpetre and mother liquor potassium silicofluoride crystallization, from mother liquor, isolate the fluorine resource; Produce required nitro azophoska compound fertilizer by in N-process or granulation process, adding the saltpetre nutrient.
The present invention realizes that the process of mid low grade phosphate rock production nitrophosphate fertilizer is: phosphorus ore and nitric acid join the acidolysis groove and carry out phosphorus ore acid hydrolysis, then after from acid hydrolysis solution, precipitating and isolating acid non-soluble substance, again acid hydrolysis solution is added the deep removal that flocculation agent carries out acid non-soluble substance, the acid hydrolysis solution that has thoroughly separated acid non-soluble substance carries out freezing and crystallizing makes nitrocalcite crystallization from acid hydrolysis solution, carry out afterwards nitrocalcite and filter, nitrocalcite is filtered the mother liquid obtained saltpetre defluorinate (SiF that adds 6 2-+ 2K +=K 2SiF 6↓), the mother liquor after defluorinate carries out ammonia neutralization, afterwards in and slip through evaporation, granulation, be drying to obtain total nutrient greater than 40% nitro azophoska compound fertilizer product, the required saltpetre nutrient of nitrogen-phosphorus-potassium compound fertilizer adds at N-process or granulation process.
The present invention has following advantage:
(1) nitro azophoska compound fertilizer of available mid low grade phosphate rock production high density;
(2) increase the acid non-soluble substance deep removal, mother liquor defluorinate operation method is simple, and is relatively independent, have a style of one's own, be easy to realize technological transformation at former Phosphate Fertilizer Nitrate with Frozen Method device;
(3) beneficial effect that defluorinate process arranges: recycled the fluorine resource on the one hand, obtained the byproduct potassium silicofluoride, reduced on the other hand the pollution of fluorine to environment;
(4) on former Phosphate Fertilizer Nitrate with Frozen Method production equipment, by adding saltpetre at N-process or granulation process, conveniently, realized simply, neatly the production of nitrogen-phosphorus-potassium compound fertilizer, the consistency that is embodied in saltpetre and nitrophosphate fertilizer technological process is good, and the ratio of nitrogen phosphorus potassium is adjustable as required in the nitro-compound fertilizer;
(5) products obtained therefrom good physical and chemical, not chloride, applied widely, shape is the particulate state prevented from caking, has the very strong market competitiveness.
Utilize mid low grade phosphate rock to produce the inexorable trend that nitrogen-phosphorus-potassium compound fertilizer is China's development nitrophosphate fertilizer, and the ripe of development low-grade phosphate ore production high-quality nitrogen-phosphorus-potassium compound fertilizer, the enforcement of high density defluorinate nitro azophoska compound fertilizer production method of the present invention can be the long term growth of nitrophosphate fertilizer industry and lays a good foundation.
Description of drawings
The process flow diagram of the embodiment of Fig. 1, high density defluorinate nitro azophoska compound fertilizer of the present invention.
Among the above-mentioned figure:
1-phosphorus ore 2-nitric acid, 3-acidolysis reaction, 4-precipitate and separate 5-acid non-soluble substance
6-acid non-soluble substance deep removal, 7-flocculation agent, 8-solid-liquid separation, 9-acid non-soluble substance
10-freezing and crystallizing, 11-nitre calcium filters 12-nitrocalcite 13-mother liquor
14-mother liquor defluorinate, 15-saltpetre, 16-solid-liquid separation, 17-potassium silicofluoride
The neutralization of 18-saltpetre, 19-ammonium nitrate, 20-ammonia, 21-mother liquor
The cooling of 22-slip evaporation, 23-slurry granulation, 24-dry materials, 25-material
26-nitro azophoska compound fertilizer
Embodiment
Below in conjunction with embodiment and accompanying drawing thereof the specific embodiment of the present invention is described in detail, but they are not limitation of the invention.
Technical process explanation of the present invention:
Present embodiment is on the basis of the known Phosphate Fertilizer Nitrate with Frozen Method technological process of production, increased acid non-soluble substance deep removal process 6 in acid non-soluble substance precipitate and separate step, increased mother liquor defluorinate 14 operations between nitrocalcite filtration and two steps of mother liquor neutralization, Fig. 1 is seen in its technical process.Nitric acid 2 and phosphorus ore 1 are added to by stoichiometry and carry out acidolysis reaction 3 in the acidolysis groove, acid non-soluble substance 5 in the acid hydrolysis solution carries out initial gross separation through precipitate and separate 4, acid hydrolysis solution after the separation enters in the acid non-soluble substance deep removal operation 6, by adding flocculation agent 7 acid non-soluble substance 9 is carried out deep removal through solid-liquid separation 8, the acid hydrolysis solution that then will thoroughly separate acid non-soluble substance is sent into freezing and crystallizing 10, separate out and enter nitrocalcite filtration 11 through freezing and crystallizing nitrocalcite 12 from acid hydrolysis solution and carry out solid-liquid separation, gained liquid is mother liquor 13; Will be through mother liquor defluorinate 14 operations before 20 neutralizations of mother liquor 13 usefulness ammonias, to filter 11 mother liquor 13 from nitrocalcite delivers in the mother liquor defluorinate groove, carry out the mother liquor defluorinate by adding saltpetre 15, make silicofluoric acid ion and potassium ion reaction in the mother liquor 13 generate potassium silicofluoride crystallization 17; Technique according to Phosphate Fertilizer Nitrate with Frozen Method neutralizes at N-process adding ammonia 20 and ammonium nitrate 19, in order to obtain nitrogen-phosphorus-potassium compound fertilizer 26 products, also to add the saltpetre 18 of calculated amount at N-process, then successively through evaporate 22, granulation 23, dry 24, cooling 25 make defluorinate nitro azophoska compound fertilizer 26.
In order to obtain nitrogen-phosphorus-potassium compound fertilizer 26 products, the saltpetre 18 of the calculated amount that present embodiment is required also can be added into granulating working procedure 23.
Embodiment one
The quality index of the phosphorus ore 1 of present embodiment: P 2O 527%, CaO 42%, AI 18%, F 2.9%, MgO 2%, Fe 2(Al 2O) 3Total 3%, other impurity; The concentration of nitric acid 2 is 58%.
Nitric acid 2 and phosphorus ore 1 are added to by stoichiometry 1.2:1 and carry out acidolysis reaction 3 in the acidolysis groove, acid non-soluble substance 5 in the acid hydrolysis solution carries out initial gross separation through precipitate and separate 4, acid hydrolysis solution after the separation enters in the acid non-soluble substance deep removal operation 6, carry out acid non-soluble substance deep removal 6 by adding flocculation agent 7, flocculation sediment 0.5-1 hour separates 8 with acid non-soluble substance 9 deep removals by solid-liquid filtration, thoroughly separate the acid hydrolysis solution of acid non-soluble substance and sent into freezing and crystallizing 10, separate out and enter nitrocalcite filtration 11 through freezing and crystallizing nitrocalcite 12 from acid hydrolysis solution and carry out solid-liquid separation, gained liquid is mother liquor 13; Another feature of present embodiment is that 20 neutralizations of mother liquor 13 usefulness ammonias before will be through mother liquor defluorinate 14 operations, to filter 11 mother liquor 13 from nitrocalcite delivers in the mother liquor defluorinate groove, carry out the mother liquor defluorinate by adding saltpetre 15, make silicofluoric acid ion and potassium ion reaction in the mother liquor 13 generate potassium silicofluoride crystallization 17, the process reaction condition is 10-50 ℃ of temperature of reaction, in 0.5-1 hour reaction times, the add-on of saltpetre 15 according to the mol ratio of saltpetre and silicofluoric acid is: KNO 3/ H 2SiF 6=2-4; Technique adding ammonia 20 and the ammonium nitrate 19 of mother liquor after the degree of depth defluorinate according to Phosphate Fertilizer Nitrate with Frozen Method is neutralized, the addition of ammonia is 0.10-15 with the phosphorus ore quality ratio, the addition of ammonium nitrate is 0.12-0.20 with the phosphorus ore quality ratio, in order to obtain nitrogen-phosphorus-potassium compound fertilizer 26 products, also to add the saltpetre 18 of calculated amount at N-process, the addition of saltpetre is 0.2-0.4 with the phosphorus ore quality ratio, then successively through evaporate 22, granulation 23, dry 24, cooling 25 make nitro azophoska compound fertilizer 26.
In order to obtain nitrogen-phosphorus-potassium compound fertilizer 26 products, the saltpetre 18 of the calculated amount that present embodiment is required also can be added into granulating working procedure.
The total nutrient concentration of present embodiment gained nitrogen-phosphorus-potassium compound fertilizer 26 products 〉=40% wherein contains P 2O 512.3%, N 22%, K 2O 7%, other nutrients 2%, other nutrients refer to trace element such as calcium, magnesium, sulphur, aluminium, iron, manganese etc.
Embodiment two
The quality index of the phosphorus ore 1 of present embodiment is different from embodiment's one, and quality index is: P 2O 522%, CaO 45%, AI 18.7%, F 2.5%, MgO 2.0%, Fe 2(Al 2O) 3Total 3.2%, other impurity; The concentration of nitric acid 2 is 58%.
Other processes are identical with the production process of embodiment one defluorinate high density nitro azophoska compound fertilizer.
The total nutrient concentration of present embodiment gained nitrogen-phosphorus-potassium compound fertilizer 26 products 〉=40% wherein contains P 2O 511%, N 20%, K 2O 7%, other nutrients 2.0%.

Claims (6)

1. the production method of a defluorinate high density nitro azophoska compound fertilizer, be based on the operational path of existing Phosphate Fertilizer Production, comprise following successively step: phosphorus ore adds nitric acid solution, acid non-soluble substance precipitate and separate, nitrocalcite freezing and crystallizing, nitrocalcite filtration, mother liquor neutralization, evaporation, granulation, dry and cooling, it is characterized in that: increased acid non-soluble substance deep removal step in acid non-soluble substance precipitate and separate step, between nitrocalcite filtration and two steps of mother liquor neutralization, increased mother liquor defluorinate step.
2. the production method of a kind of defluorinate high density nitro azophoska compound fertilizer according to claim 1, it is characterized in that: described acid non-soluble substance deep removal step comprises following process:
1) precipitate and separate process: acid hydrolysis solution is precipitated, filters, make the acid non-soluble substance in the acid hydrolysis solution carry out preliminary separation;
2) acid non-soluble substance deep removal process: to initial gross separation the acid hydrolysis solution of acid non-soluble substance add flocculation agent, then flocculation sediment 0.5-1 hour carries out filtration treatment, the acid hydrolysis solution that has removed acid non-soluble substance is sent to the nitrocalcite freezing and crystallizing.
3. the production method of a kind of defluorinate high density nitro azophoska compound fertilizer according to claim 1, it is characterized in that: described mother liquor defluorinate step comprises following process:
1) defluorinate process: add saltpetre to mother liquor, make silicofluoric acid ion and potassium ion reaction in the mother liquor generate the potassium silicofluoride crystallization, the process reaction condition is 10-50 ℃ of temperature of reaction, 0.5-1 hour reaction times, the add-on of saltpetre is pressed the silicofluoric acid content in the mother liquor and is decided, and namely the mol ratio of saltpetre and silicofluoric acid is: 2-4;
2) solid-liquid separation process: the slip behind the defluorination reaction is separated by filtration out the solid phase prod potassium silicofluoride, and filtrate is the defluorinate mother liquor, is sent in next step and operation.
4. the production method of a kind of defluorinate high density nitro azophoska compound fertilizer according to claim 1, it is characterized in that: add saltpetre and ammonium nitrate to adjust the nitrogen phosphoris and potassium fertilizer ratio of fertilizer product at the mother liquor N-process, the addition of saltpetre is 0.2-0.4 with the phosphorus ore quality ratio, and the addition of ammonium nitrate is 0.12-0.20 with the phosphorus ore quality ratio.
5. the production method of a kind of defluorinate high density nitro azophoska compound fertilizer according to claim 4, it is characterized in that: the saltpetre that adds also can add at granulation process.
6. the production method of a kind of defluorinate high density nitro azophoska compound fertilizer according to claim 1, it is characterized in that: add in the nitric acid solution process at phosphorus ore, described phosphorus ore is mid low grade phosphate rock, wherein P 2O 521%-30wt%, MgO≤2.0wt%, Fe 2(Al 2O) 3≤ 3.5wt %, F≤3.0wt%, AI≤20wt%.
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CN103524150A (en) * 2013-09-27 2014-01-22 深圳市芭田生态工程股份有限公司 Method and device for producing granular nitric phosphateby decomposing phosphate ore through nitric acid
CN104108969A (en) * 2014-07-04 2014-10-22 贵州芭田生态工程有限公司 Granulation method of phosphorus-potassium nitrate fertilizer
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CN103524150A (en) * 2013-09-27 2014-01-22 深圳市芭田生态工程股份有限公司 Method and device for producing granular nitric phosphateby decomposing phosphate ore through nitric acid
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CN104108969A (en) * 2014-07-04 2014-10-22 贵州芭田生态工程有限公司 Granulation method of phosphorus-potassium nitrate fertilizer
CN104211485A (en) * 2014-09-17 2014-12-17 中化化肥有限公司重庆磷复肥工程技术研究中心 Method for producing crystalline potassium dihydrogen phosphate and potassium nitrate macroelement water-soluble fertilizer
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CN105272441A (en) * 2015-09-23 2016-01-27 四川泸天化股份有限公司 Process for production of liquid compound fertilizer by combination of decomposition of phosphate ore by use of nitric acid and removal of calcium by use of potassium salt
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CN112758937A (en) * 2021-01-14 2021-05-07 襄阳泽东化工集团有限公司 Method for preparing potassium fluosilicate and NPK compound fertilizer from phosphorus-potassium associated ore
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