CN102126741B - Method for producing nitro/S-based compound fertilizer and coproducing plaster - Google Patents
Method for producing nitro/S-based compound fertilizer and coproducing plaster Download PDFInfo
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- CN102126741B CN102126741B CN2011100222234A CN201110022223A CN102126741B CN 102126741 B CN102126741 B CN 102126741B CN 2011100222234 A CN2011100222234 A CN 2011100222234A CN 201110022223 A CN201110022223 A CN 201110022223A CN 102126741 B CN102126741 B CN 102126741B
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Abstract
The invention provides a method for producing a nitro/S-based compound fertilizer and coproducing plaster, belonging to the technical field of compound fertilizer production. The method comprises the following steps: after decomposing phosphorite with nitric acid, firstly filtering and removing the acid insoluble matters and organic suspended matters; adding industrial ammonium sulfate or sulfuric acid to the purified acidolysis solution to remove calcium and filtering the reaction solution to obtain the calcium removed byproduct, namely high-purity plaster, wherein the acidolysis solution after calcium removal is used for producing the nitro/S-based compound fertilizer; and mixing the calcium removed acidolysis solution with acid potassium sulfate to form mixed acid, subjecting the mixed acid to carry out neutralization reaction with ammonia to obtain slurry containing ammonium nitrate, monoammonium phosphate, ammonium sulfate and potassium sulfate and pelleting and drying the slurryto obtain the nitro/S-based compound fertilizer. The method has the following beneficial effects: the ammonium sulfate or sulfuric acid is used for removing calcium from the acidolysis solution obtained after decomposing phosphorite with the nitric acid, without bringing other foreign ions, and ammonia in the ammonium sulfate when the ammonium sulfate is used for removing calcium is retained in the finished product as nutrient; and the calcium removal rate of the acidolysis solution is high and is more than 95%.
Description
Technical field:
The present invention relates to a kind of nitric acid decomposing phosphate rock and produce the method for nitrate-based compound fertilizer by-product high purity gypsum, belong to composite fertilizer's production technical field, the method that is specifically related to nitric acid decomposing phosphate rock production composite fertilizer and produces high purity gypsum.
Background technology:
Sulphur (chlorine) base composite fertilizer that contains nitric nitrogen is called nitrate-based compound fertilizer.The principal feature that the nitric acid decomposing phosphate rock prepares compound fertilizer technology is that nitric acid has played dual function: both utilized the strongly-acid of nitric acid to come decomposing phosphate rock to produce phosphoric acid; Replaced the sulfuric acid decomposing phosphate rock; Practiced thrift sulfuric acid; Itself stays its negatively charged ion in the product as the nitric nitrogen nutrient again, the utilization of fullest chemical reactant.
With the technology of nitric acid decomposing phosphate rock production composite fertilizer abroad as Europe and FSU employing be cold method.China uses cold method explained hereafter nitro-compound fertilizer that a family of a day ridge Coal Chemical Industry group company (former Shanxi fertilizer plant) is only arranged, and is to have introduced Norsk Hydro cold method nitrophosphate fertilizer device from Norway.This device is because of using the phosphorus ore production that domestic grade is low, foreign matter content is high, and nitrocalcite cold method separation difficulty still exists a lot of problems not solve at present on the technology, cause only this cover of domestic cold method nitrophosphate fertilizer device.The defective of this technology is huge, the long flow path of plant investment, to ingredient requirement harshness, complicated operation, the domestic phosphorus ore of device incompatibility etc.
Document 1 Chinese patent " a kind of process method of producing high concentration nitric-phosphate fertilizer " (application number: 200910009223.3); It comprises the steps: that 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; Between nitrocalcite filtration and mother liquor neutralization, mother liquor degree of depth deliming step is arranged; This step comprises following process: I) the mother liquor degree of depth is removed mother liquor of calcium interpolation sulfuric acid or ammonium sulfate, and the calcium ion of mother liquor and sulfate ion generate the terra alba crystallization; II) the reaction slurry stage treatment adopts stage equipment that reaction slurry is carried out stage treatment, and the reaction slurry that has small-particle calcium sulfate returns the deliming of the mother liquor degree of depth, and the reaction slurry that has macrobead calcium sulfate is delivered to the calcium sulfate filtration; III) calcium sulfate filtering reaction slip filters and washing through filter, and during just a filtrating and a washing lotion are sent to and operation, two washing lotions are returned filter.
Document 2 Chinese patents " a kind of nitric acid decomposing rock phosphate with hydrogen is produced the method and the system thereof of nitro-compound fertilizer material " (application number: 200810215546.3); This method is a kind of method and system of preparing sulphur based compound fertilizer by decomposing rock phosphate with hydrogen nitrate; Its step is following: the preparation of (1) sal enixum gets nitration mixture I; (2) nitric acid decomposing rock phosphate with hydrogen gets nitration mixture II; (3) nitration mixture I mixes with nitration mixture II; (4) with step (3) gained nitration mixture III and liquefied ammonia or gas ammonia reaction, get sulphur based compound fertilizer.
Above-mentioned existing method is all with the nitric acid decomposing phosphate rock and prepares the relevant working method of composite fertilizer, has close with the present invention or the part that communicates.But existing cold method technology is had relatively high expectations to phosphorus ore grade and foreign matter content, and freezing to remove nitrocalcite incomplete, and the decalcification rate is about 75%～80%; The nitrocalcite of by-product needs metathesis to produce lime carbonate; This technology can not be produced NPK composite fertilizer, and flow operations is complicated, invests huge.
The method of document 1 is the improvement to existing cold method nitrophosphate fertilizer technology; Increased with sulfuric acid and ammonium sulfate degree of depth decalcification process, but the crystal of calcium sulfate that removes is tiny, needs classification is carried out in crystallization; Mother liquor circulates in a large number, also will carry out metathesis to isolated calcium sulfate and be converted into lime carbonate.This technology can not be produced NPK composite fertilizer equally, and flow operations is complicated more, invests bigger.
In the method for document 2, sal enixum (nitration mixture I) is mixed with the acid hydrolysis solution (nitration mixture II) of nitric acid decomposing phosphate rock, make sulfate ion and the production of the calcium ion among nitration mixture II calcium sulfate precipitation among the nitration mixture I remove the calcium in the feed liquid.But this decalcification method is owing to there is the existence of potassium ion, the hydrofluoric acid in the acid hydrolysis solution can with its generation metathesis side reaction, produce insoluble potassium silicofluoride.Remove acid non-soluble substance, the organic seston contain behind the phosphorus ore acid hydrolysis in the calcium sulfate filtrate that this method is come out, also contain the potassium silicofluoride that side reaction produces.On the one hand calcium sulfate precipitation is carried secretly with the potassium silicofluoride deposition and is taken away nutrient potassium, causes the loss of potassium, and the calcium sulfate impurity that comes out of this method is numerous on the other hand, can't further utilize, and can only stack as phosphogypsum.
Summary of the invention:
The object of the invention; The shortcoming that be to overcome that existing cold method nitrophosphate fertilizer technical process complicated operation, investment are huge, the acid hydrolysis solution decalcification by-product calcium sulfate precipitation foreign matter content height of the shortcoming that can not produce NPK composite fertilizer and existing nitric acid decomposing phosphate rock can't fully utilize provides a kind of method of producing the nitrate-based compound fertilizer by-product gypsum.
The present invention realizes like this: behind the nitric acid decomposing phosphate rock; Earlier acid non-soluble substance and organic seston are removed by filter; Acid hydrolysis solution after the purification adds industrial sulphuric acid ammonium or sulfuric acid decalcification, filters to obtain decalcification sub product high purity gypsum, and the acid hydrolysis solution after the decalcification is used for producing nitrate-based compound fertilizer again.
A kind of method of producing the nitrate-based compound fertilizer by-product gypsum specifically may further comprise the steps:
(1) with carrying out acidolysis reaction with nitric acid behind the phosphorus ore grinding;
(2) the thick acid hydrolysis solution that step (1) is obtained filters, and removes wherein acid non-soluble substance and organic seston, and filtrating is smart acid hydrolysis solution;
(3) smart acid hydrolysis solution adding ammonium sulfate or the sulfuric acid with step (2) carries out the replacement(metathesis)reaction decalcification, and reaction solution is filtered, and solid is a high purity gypsum, after the washing drying, is gypsum product, and filtrating is the decalcification acid hydrolysis solution;
(4) with the decalcification acid hydrolysis solution in the step (3) with become nitration mixture after sal enixum mixes, nitration mixture and gas ammonia neutralization reaction must contain the slip of an ammonium nitrate, monoammonium phosphate, ammonium sulfate, vitriolate of tartar, slip obtains nitrate-based compound fertilizer through granulation, drying.
Foregoing method, preferably scheme is, and the nitric acid mass concentration is 40-70% in the step (1), and the optimization mass concentration is 55-65%, more optimizes 60%.
Foregoing method, preferred scheme be, the mol ratio 1 of calcium ion and nitric acid in phosphorus ore when step (1) is carried out acidolysis reaction: 2-3 is optimized for 1: 2-2.3.
Foregoing method, preferred scheme is that temperature of reaction was 45-70 ℃ when step (1) was carried out acidolysis reaction, was optimized for 55-60 ℃, more optimized 58 ℃.
Foregoing method, preferably scheme is, and it is 0.5-4 hour that step (1) is carried out the acidolysis reaction the reaction time, and optimal conditions is 1-2 hour.
Foregoing method, preferred scheme is that ammonium sulfate or sulfuric acid add-on are pressed the mol ratio 1-1.2 of calcium ion in sulfate ion and the smart acid hydrolysis solution in the step (3): 1.
Foregoing method, preferred scheme is that temperature of reaction was 55-60 ℃ when step (3) was carried out metathesis.
Foregoing method, preferred scheme is that it is 1-4 hour that step (3) is carried out the metathesis the reaction time, is optimized for 2-2.5 hour.
Foregoing method, preferred scheme is that the granulation mode is spray granulating, ammoniation-granulation, high tower pellatizer or biaxial granulation in the step (4).
Produce in the method for nitrate-based compound fertilizer by-product gypsum in the present invention, the add-on of sal enixum is allocated into by NPK content ratio requirement in the product in the step (4).Such as: to the product of potassium content at 8-10%, the add-on of sal enixum is the 23-30% of decalcification acid hydrolysis solution weight.
A kind of method of producing the nitrate-based compound fertilizer by-product gypsum, another technical thought are that the gained slip is produced powder-like product without granulation with the spraying drying mode in the step (4).
The present invention has following characteristic and beneficial effect:
(1) the present invention first filter acid insolubles and organic seston before the acid hydrolysis solution decalcification of nitric acid decomposing phosphate rock; Decalcification sub product terra alba (gypsum) purity is reached more than 99%; Can be used as high purity gypsums such as mould gypsum, medical gypsum, filler; No phosphogypsum discharging realizes the comprehensive utilization of resource;
(2) acid hydrolysis solution of phosphorolytic cleavage phosphorus ore of the present invention removes calcium and uses ammonium sulfate or sulfuric acid, is not with other foreign ions of people, and the ammonia during with the ammonium sulfate decalcification in the ammonium sulfate is stayed in the finished product as nutrient;
(3) decreasing ratio of acidolysis liquid calcium of the present invention is high, arrives more than 95%, and this is that cold method technology is incomparable;
(4) the present invention does not have freezing in the cold method technology, nitrocalcite to be converted into operations such as lime carbonate, simplified control, and investment significantly reduces;
(5) the present invention can produce the nitrate-based compound fertilizer that contains NPK.
Embodiment:
Specify technical scheme of the present invention below in conjunction with embodiment, but protection domain is not by this restriction.
Raw materials usedly among the embodiment all can buy from market, used sal enixum is with Repone K and the sulfuric acid sal enixum (but reference 3 Chinese patents " working method of potassium sulphate type ternary composite fertilizer ") through the low temperature conversion preparation in the production of sulfur-based compound fertilizer
Embodiment 1: implement raw material: 1, ground phosphate rock: P
20
5Content is 30.72%, and CaO is 48.28%; 2, nitric acid: concentration 70%; 3, industrial sulphuric acid ammonium: ammonia content 21%.
Implementation process of the present invention may further comprise the steps:
(1) after being added water, ground phosphate rock carries out acidolysis reaction, the mol ratio 1: 3 of calcium ion and nitric acid in the phosphorus ore with 70% nitric acid; Temperature of reaction is 45 ℃, reacts 0.5 hour.
(2) the thick acid hydrolysis solution that step (1) is obtained filters, and removes wherein acid non-soluble substance and organic seston, and filtrating is smart acid hydrolysis solution.
(3) the smart acid hydrolysis solution of step (2) is added the industrial sulphuric acid ammonium and carry out replacement(metathesis)reaction, the ammonium sulfate add-on is pressed the mol ratio 1: 1 of calcium ion in sulfate ion and the smart acid hydrolysis solution; Temperature of reaction is 55 ℃; Reaction times is 1 hour.Reaction solution is filtered, and solid is a high purity gypsum, after the washing drying, is the high purity gypsum product; Filtrating is the decalcification acid hydrolysis solution.
(4) after being mixed, the decalcification acid hydrolysis solution in the step (3) and sal enixum (add-on of sal enixum be decalcification acid hydrolysis solution weight 23.5%) become nitration mixture; Nitration mixture and gas ammonia neutralization reaction; The slip that must contain an ammonium nitrate, monoammonium phosphate, ammonium sulfate, vitriolate of tartar, slip obtains nitrate-based compound fertilizer through spray granulating, drying.
Result of implementation: 1. high purity gypsum: the sulfate dihydrate calcium contents is 99.3% in the gypsum through detecting; 2. nitrate-based compound fertilizer: total nitrogen content 21.5%, phosphorus (P
2O
5) content is 10.0%, potassium (K
2O) content is 8.5%.
Embodiment 2: implement raw material: 1, ground phosphate rock: P
2O
5Content is 29.85%, and CaO is 48.30%; 2, nitric acid: concentration 40%; 3, industrial sulphuric acid ammonium: ammonia content 21%.
Implementation process of the present invention may further comprise the steps:
(1) after being added water, ground phosphate rock carries out acidolysis reaction, the mol ratio 1: 2 of calcium ion and nitric acid in the phosphorus ore with 40% nitric acid; Temperature of reaction is 70 ℃, reacts 4 hours.
(2) the thick acid hydrolysis solution that step (1) is obtained filters, and removes wherein acid non-soluble substance and organic seston, and filtrating is smart acid hydrolysis solution.
(3) the smart acid hydrolysis solution of step (2) is added the industrial sulphuric acid ammonium and carry out replacement(metathesis)reaction, the ammonium sulfate add-on is pressed the mol ratio 1.2: 1 of calcium ion in ammonium sulfate and the smart acid hydrolysis solution; Temperature of reaction is 60 ℃; Reaction times is 4 hours.Reaction solution is filtered, and solid is a high purity gypsum, after the washing drying, is the high purity gypsum product; Filtrating is the decalcification acid hydrolysis solution.
(4) after being mixed, the decalcification acid hydrolysis solution in the step (3) and sal enixum (add-on of sal enixum be decalcification acid hydrolysis solution weight 26%) become nitration mixture; Nitration mixture and gas ammonia neutralization reaction; The slip that must contain an ammonium nitrate, monoammonium phosphate, ammonium sulfate, vitriolate of tartar, slip obtains nitrate-based compound fertilizer through ammoniation-granulation, drying.
Result of implementation: 1, high purity gypsum: the sulfate dihydrate calcium contents is 99.5% in the gypsum through detecting; 2, nitre chlorine-based compound fertilizer: total nitrogen content 21.0%, phosphorus (P
2O
5) content is 10.0%, potassium (K
2O) content is 9.0%.
Embodiment 3: implement raw material: 1, ground phosphate rock: P
2O
5Content is 31.05%, and CaO is 47.65%; 2, nitric acid: concentration 60%; 3, industrial sulphuric acid: concentration 98%.
Implementation process of the present invention may further comprise the steps:
(1) after being added water, ground phosphate rock carries out acidolysis reaction, the mol ratio 1: 2 of calcium ion and nitric acid in the phosphorus ore with 60% nitric acid; Temperature of reaction is 50 ℃, reacts 1.5 hours.
(2) the thick acid hydrolysis solution that step (1) is obtained filters, and removes wherein acid non-soluble substance and organic seston, and filtrating is smart acid hydrolysis solution.
(3) the smart acid hydrolysis solution of step (2) is added industrial sulphuric acid and carry out replacement(metathesis)reaction, the sulfuric acid add-on is pressed the mol ratio 1.1: 1 of calcium ion in sulfate ion and the smart acid hydrolysis solution; Temperature of reaction is 60 ℃; Reaction times is 3 hours.Reaction solution is filtered, and solid is a high purity gypsum, after the washing drying, is the high purity gypsum product; Filtrating is the decalcification acid hydrolysis solution.
(4) allocate the decalcification acid hydrolysis solution in the step (3) into sal enixum (add-on of sal enixum be decalcification acid hydrolysis solution weight 23%) back and gas ammonia neutralization reaction, composite fertilizer's slip of nitrogenous phosphorus potassium.Slip obtains nitrate-based compound fertilizer through biaxial granulation, drying, screening.
Result of implementation: 1, high purity gypsum: the sulfate dihydrate calcium contents is 99.2% in the gypsum through detecting; 2, nitrate-based compound fertilizer: total nitrogen content 23.1%, phosphorus (P
2O
5) content is 9.0%, potassium (K
2O) content is 8.0%.
Embodiment 4: implement raw material: 1, ground phosphate rock: P
2O
5Content is 30.72%, and CaO is 48.28%; 2, nitric acid: concentration 65%; 3, industrial sulphuric acid ammonium: ammonia content 21%.
Implementation process of the present invention may further comprise the steps:
(1) after being added water, ground phosphate rock carries out acidolysis reaction, the mol ratio 1: 2 of calcium ion and nitric acid in the phosphorus ore with 65% nitric acid; Temperature of reaction is 58 ℃, reacts 1.5 hours.
(2) the thick acid hydrolysis solution that step (1) is obtained filters, and removes wherein acid non-soluble substance and organic seston, and filtrating is smart acid hydrolysis solution.
(3) the smart acid hydrolysis solution of step (2) is added the industrial sulphuric acid ammonium and carry out replacement(metathesis)reaction, the ammonium sulfate add-on is pressed the mol ratio 1.2: 1 of calcium ion in sulfate ion and the smart acid hydrolysis solution; Temperature of reaction is 60 ℃; Reaction times is 2 hours.Reaction solution is filtered, and solid is a high purity gypsum, after the washing drying, is the high purity gypsum product; Filtrating is the decalcification acid hydrolysis solution.
(4) allocate the decalcification acid hydrolysis solution in the step (3) into sal enixum (add-on of sal enixum be decalcification acid hydrolysis solution weight 27%) back and gas ammonia neutralization reaction, composite fertilizer's slip of nitrogenous phosphorus potassium.The spray-dried powdery nitrate-based compound fertilizer that obtains of slip.
Result of implementation: 1, high purity gypsum: the sulfate dihydrate calcium contents is 99.5% in the gypsum through detecting; 2, powdery nitrate-based compound fertilizer: total nitrogen content 21.5%, phosphorus (P
2O
5) content is 9.5%, potassium (K
2O) content is 9.0%.
Claims (9)
1. a method of producing the nitrate-based compound fertilizer by-product gypsum is characterized in that, may further comprise the steps:
(1) with carrying out acidolysis reaction with nitric acid behind the phosphorus ore grinding, used nitric acid mass concentration is 40-70%, the mol ratio 1:2-3 of calcium ion and nitric acid in the phosphorus ore when carrying out acidolysis reaction, and temperature of reaction is 45-70 ℃, the reaction times is 0.5-4 hour;
(2) the thick acid hydrolysis solution that step (1) is obtained filters, and removes wherein acid non-soluble substance and organic seston, and filtrating is smart acid hydrolysis solution;
(3) smart acid hydrolysis solution adding ammonium sulfate or the sulfuric acid with step (2) carries out the replacement(metathesis)reaction decalcification; Temperature of reaction is 55-60 ℃, and the reaction times is 1-4 hour, and reaction solution is filtered; Solid is a high purity gypsum; After the washing drying, be gypsum product, filtrating is the decalcification acid hydrolysis solution, and ammonium sulfate or sulfuric acid add-on are pressed the mol ratio 1-1.2:1 of calcium ion in sulfate ion and the smart acid hydrolysis solution;
(4) with the decalcification acid hydrolysis solution in the step (3) with become nitration mixture after sal enixum mixes, nitration mixture and gas ammonia neutralization reaction must contain the slip of an ammonium nitrate, monoammonium phosphate, ammonium sulfate, vitriolate of tartar, slip obtains nitrate-based compound fertilizer through granulation, drying.
2. method according to claim 1 is characterized in that, the nitric acid mass concentration is 55-65% in the step (1).
3. method according to claim 2 is characterized in that, the nitric acid mass concentration is 60%.
4. method according to claim 1 is characterized in that, when step (1) is carried out acidolysis reaction in the phosphorus ore mol ratio of calcium ion and nitric acid be 1:2-2.3.
5. method according to claim 1 is characterized in that, temperature of reaction was 55-60 ℃ when step (1) was carried out acidolysis reaction.
6. method according to claim 5 is characterized in that, temperature of reaction is 58 ℃.
7. method according to claim 1 is characterized in that, it is 1-2 hour that step (1) is carried out the acidolysis reaction the reaction time.
8. method according to claim 1 is characterized in that, it is 2-2.5 hour that step (3) is carried out the metathesis the reaction time.
9. method according to claim 1 is characterized in that, the granulation mode is spray granulating, ammoniation-granulation, high tower pellatizer or biaxial granulation in the step (4).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104108968B (en) * | 2014-07-04 | 2017-10-03 | 贵州芭田生态工程有限公司 | A kind of granulation process of nitrophosphate fertilizer |
| CN106396915A (en) * | 2016-08-31 | 2017-02-15 | 宜昌富升化工有限公司 | Fully water-soluble nitro-sulfur based composite fertilizer and preparation method thereof |
| CN111533154B (en) * | 2020-04-21 | 2023-06-02 | 贵州大学 | Method for decomposing phosphate rock acidolysis solution by nitric acid to remove calcium and obtain byproduct alpha high-strength gypsum |
| CN111533099B (en) * | 2020-05-22 | 2021-12-07 | 四川大学 | Production method of water-soluble monoammonium phosphate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280111A (en) * | 1999-07-13 | 2001-01-17 | 李守义 | Middle concentrate compound potassium sulfate fertilizer and its producing method |
| CN101343200A (en) * | 2008-09-09 | 2009-01-14 | 中国-阿拉伯化肥有限公司 | Method for preparing sulphur based compound fertilizer by decomposing rock phosphate with hydrogen nitrate and system thereof |
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| JP2000143378A (en) * | 1998-11-05 | 2000-05-23 | Asahi Chem Ind Co Ltd | Porous compound fertilizer |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1280111A (en) * | 1999-07-13 | 2001-01-17 | 李守义 | Middle concentrate compound potassium sulfate fertilizer and its producing method |
| CN101343200A (en) * | 2008-09-09 | 2009-01-14 | 中国-阿拉伯化肥有限公司 | Method for preparing sulphur based compound fertilizer by decomposing rock phosphate with hydrogen nitrate and system thereof |
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| JP特开2000-143378A 2000.05.23 |
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