CN115385319A - Method for producing magnesium ammonium phosphate slow-release fertilizer by wet-process phosphoric acid - Google Patents
Method for producing magnesium ammonium phosphate slow-release fertilizer by wet-process phosphoric acid Download PDFInfo
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- CN115385319A CN115385319A CN202210996544.2A CN202210996544A CN115385319A CN 115385319 A CN115385319 A CN 115385319A CN 202210996544 A CN202210996544 A CN 202210996544A CN 115385319 A CN115385319 A CN 115385319A
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- Prior art keywords
- phosphoric acid
- wet
- ammonium phosphate
- magnesium ammonium
- release fertilizer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
- C01B25/451—Phosphates containing plural metal, or metal and ammonium containing metal and ammonium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/10—Compounds containing silicon, fluorine, and other elements
- C01B33/103—Fluosilicic acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/04—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
- C05B11/10—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using orthophosphoric acid
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention provides a method for producing magnesium ammonium phosphate slow-release fertilizer by wet-process phosphoric acid. The method takes wet-process phosphoric acid as a raw material, and obtains sodium fluosilicate products, particularly removes heavy metal and fluorine in polluted soil while obtaining the magnesium ammonium phosphate slow-release fertilizer by a heavy metal removing step, a fluorine removing step, a liquid ammonia adding neutralization step, a vacuum flash evaporation concentration step, a magnesium oxide powder adding neutralization step and a standing curing step.
Description
Technical Field
The invention relates to a method for producing magnesium ammonium phosphate, in particular to a method for producing magnesium ammonium phosphate slow-release fertilizer by using wet-process phosphoric acid, belonging to the technical field of chemical industry.
Background
Although the modern agriculture does not need to open a phosphate fertilizer, the phosphate fertilizer can greatly improve the yield of crops, but because heavy metal, fluorine and other metal elements in the phosphate fertilizer can cause serious pollution to soil and the pollution of phosphorus to the water environment is more and more serious, the modern agriculture advocates the use of the novel low-heavy metal, low-fluorine and low-metal element magnesium ammonium phosphate slow-release fertilizer, so as to solve the problems in the prior art. The popularization and use of the magnesium ammonium phosphate slow release fertilizer can solve the problem of phosphorus surface source pollution of soil and water environment, and can also reduce the usage amount of phosphate fertilizer to the maximum extent so as to protect increasingly exhausted phosphorus resources. Although the applicant has developed a method for producing struvite using a byproduct from the production of industrial-grade monoammonium phosphate or agricultural-grade monoammonium phosphate, the yield of the former is extremely limited, and the latter is relatively expensive, and thus cannot sufficiently meet the market demand for struvite.
Disclosure of Invention
The invention aims to provide a method for producing magnesium ammonium phosphate slow-release fertilizer, which has the advantages of simple process, wide raw material adaptability, low energy consumption, low production cost and good product quality.
The invention utilizes low-concentration wet-process phosphoric acid and adopts the process steps of heavy metal removal and defluorination to produce the high-quality magnesium ammonium phosphate slow-release fertilizer, aims to produce the high-quality magnesium ammonium phosphate slow-release fertilizer with lower energy consumption and production cost, solves the problem of environmental pollution caused by heavy metal, fluorine and phosphorus, solves the problem of excessive development of phosphorite resources, and meets the increasing demand of the market on the high-quality magnesium ammonium phosphate slow-release fertilizer.
The invention is realized by the following technical scheme: a method for producing magnesium ammonium phosphate slow release fertilizer by wet-process phosphoric acid comprises the following steps:
A. adding sodium sulfide into low-concentration wet-process phosphoric acid according to the mass ratio of 0.05-0.1%, stirring and reacting for 60-100 minutes at normal temperature, removing heavy metals, settling or filtering to obtain phosphoric acid liquid without heavy metals and filter residues, and using the filter residues for another purpose; the wet process phosphoric acid is P 2 O 5 Wet process phosphoric acid with mass concentration of 15-25%;
B. in the above-mentionedAdding sodium carbonate or sodium hydroxide into phosphoric acid solution for removing heavy metals according to the molar ratio of Na to F =1:2-3 in wet-process phosphoric acid, reacting for 60-100 minutes under normal temperature stirring, defluorinating, filtering to obtain defluorinated phosphoric acid solution and filter residue, washing the filter residue until no acid smell exists, and drying to obtain a sodium fluosilicate product, wherein: na (Na) 2 SiF 6 The content is 98.10 percent, and washing water is merged into the defluorinated phosphoric acid solution;
C. adding liquid ammonia into the defluorinated phosphoric acid solution at normal temperature until the pH value is 4.5-5.0, and carrying out neutralization exothermic reaction to preheat the slurry to obtain hot monoammonium phosphate slurry;
D. carrying out vacuum flash evaporation on the hot monoammonium phosphate slurry, and evaporating water in the reaction slurry to obtain monoammonium phosphate slurry with the water content of less than 50%;
E. adding magnesium oxide powder into the monoammonium phosphate slurry according to the molar ratio of water-soluble phosphorus to MgO of 1:1-1.4, and performing neutralization exothermic reaction to obtain an ammonium magnesium phosphate semi-finished product;
F. and standing and curing the semi-finished product of magnesium ammonium phosphate, curing the semi-finished product of magnesium ammonium phosphate into loose blocks, and crushing or granulating the loose blocks to obtain the magnesium ammonium phosphate slow release fertilizer.
Optionally, the sodium sulfide added in the step a, the sodium carbonate or sodium hydroxide added in the step B, and the liquid ammonia added in the step C are all industrial-grade products.
Optionally, the magnesia powder added in E is light-burned magnesia powder with magnesia content of more than 60%.
Optionally, in the F, the curing time is 15-30 days.
Optionally, in the step D, the hot monoammonium phosphate slurry is subjected to vacuum flash evaporation to obtain monoammonium phosphate slurry with a water content of 48% or less.
Compared with the prior art, the invention has the following advantages and effects:
1. the low-grade phosphorite, especially the high-magnesium low-grade phosphorite which is considered to be not suitable for producing wet-process phosphoric acid, and the residual acid extracted by high impurities generated by the process of extracting and purifying phosphoric acid by using a solvent can be fully utilized to produce the magnesium ammonium phosphate slow-release fertilizer, so that the resource utilization rate is enlarged, the excessive exploitation amount of the high-grade phosphorite is reduced, and the phosphorite resource is protected;
2. the magnesium ammonium phosphate slow release fertilizer with low heavy metal content and low fluorine content, which is urgently needed by the market, is produced with lower cost;
3. the reaction heat generated by the reaction of the liquid ammonia and the phosphoric acid liquid is fully utilized to preheat the slurry, so that the heat energy consumption during concentration is greatly reduced when the vacuum flash evaporation is carried out on the hot slurry, and the purpose of saving heat energy is achieved;
4. the reaction heat generated by the neutralization exothermic reaction of the ammonium phosphate slurry and the magnesium oxide is fully utilized to evaporate the moisture in the reaction slurry, thereby achieving the purpose of further saving energy consumption;
5. fluorine in the wet-process phosphoric acid is effectively recovered to form a sodium fluosilicate product, and meanwhile, the fluorine pollution to the environment caused by the fluorine contained in the phosphate fertilizer is avoided;
6. a large amount of free water is converted into solid crystal water in the curing process of magnesium ammonium phosphate ingeniously, and the drying process in the later period is omitted, so that the process is simplified, and energy is further saved and consumption is reduced.
7. The method is adopted to obtain the magnesium ammonium phosphate slow-release fertilizer and simultaneously obtain a sodium fluosilicate product, particularly to remove heavy metal and fluorine in polluted soil, solves the problem of environmental pollution caused by heavy metal and fluorine contained in the existing phosphate fertilizer, simultaneously obtains at least two products, realizes the maximum utilization of resources, has low requirement on raw materials, has wide adaptability, protects phosphate rock resources, has simple process, small equipment investment and good product quality, fully utilizes the heat energy generated by the reaction to reduce the energy consumption of concentration and drying, utilizes the mechanism that part of free water of magnesium ammonium phosphate is converted into solid crystal water during curing, saves the subsequent drying process, reduces the production cost to the minimum and has high product cost performance.
Detailed Description
The present invention will be further described with reference to the following examples.
Example one
A method for producing magnesium ammonium phosphate slow release fertilizer by wet-process phosphoric acid comprises the following steps:
step A, taking 8000 g of wet-process diluted phosphoric acid of a certain phosphate fertilizer plant, wherein: p 2 O 5 22.11％，F 1.40％，SO 3 2.03％，CaO 0.27％，MgO 1.31％，Fe 2 O 3 0.97％，AL 2 O 3 0.42 percent, adding 4.0 grams of industrial-grade sodium sulfide, reacting for 1 hour under stirring at normal temperature, removing heavy metals, filtering and separating 8002 grams of phosphoric acid liquid with heavy metals removed and 1.1 grams of filter residue, and using the filter residue as another component;
and step B, adding 125 g of industrial-grade sodium carbonate into 8002 g of the heavy metal-removed phosphoric acid solution obtained in the step A, fully reacting for 1 hour under normal temperature stirring, removing fluorine, filtering and separating to obtain 7815 g of filtrate and 261 g of filter residue, washing the filter residue with 200 g of water in a fractional manner until no acid smell exists, and drying to obtain 145 g of sodium fluosilicate product, wherein: na (Na) 2 SiF 6 The content is 98.10%, and washing liquid is merged into the filtrate in the step to obtain 8041 g of defluorinated phosphoric acid liquid; through the steps, fluorine in the wet-process phosphoric acid can be effectively recovered to form a sodium fluosilicate product, and meanwhile, the fluorine pollution to the environment caused by the fluorine contained in the phosphate fertilizer is avoided;
step C, adding liquid ammonia into 8041 g of defluorinated phosphoric acid solution obtained in the step B at normal temperature until the pH value is 4.9, and carrying out neutralization exothermic reaction to preheat the slurry to obtain 8490 g of hot monoammonium phosphate slurry, so that the heat energy consumption during concentration is greatly reduced when the hot slurry is subjected to vacuum flash evaporation and evaporation, and the purpose of saving heat energy is achieved;
d, performing vacuum flash evaporation on the hot monoammonium phosphate slurry obtained in the step C according to a conventional method, and evaporating water in the reaction slurry to obtain 6989 g of monoammonium phosphate slurry with the water content of 45.0%;
step E, adding 1420 g of light-burned magnesia powder into the monoammonium phosphate slurry obtained in the step D, wherein the MgO content is 73.30%, carrying out neutralization exothermic reaction to obtain an ammonium magnesium phosphate semi-finished product, evaporating water in the reaction slurry, and further achieving the purpose of saving energy consumption;
and F, standing and curing the semi-finished product of magnesium ammonium phosphate obtained in the step E for 15 days, curing the semi-finished product of magnesium ammonium phosphate into loose blocks, and conventionally crushing the loose blocks to obtain 7072 g of magnesium ammonium phosphate slow release fertilizer, wherein: available phosphorus P 2 O 5 25.08 percent, 15.30 percent of MgO and 5.03 percent of N. In the step, a large amount of free water is ingeniously converted into solid in the curing process of magnesium ammonium phosphateThe crystal water is crystallized, and the drying process in the later period is saved, so that the process is simplified, the energy is further saved, and the consumption is reduced.
Example two
Step A, taking 8000 g of wet-process diluted phosphoric acid of a certain phosphate fertilizer plant, wherein: p 2 O 5 21.56％，F 1.52％，SO 3 2.01％，CaO 0.23％，MgO 0.95％，Fe 2 O 3 0.86％，AL 2 O 3 0.38 percent, adding 6.0 grams of industrial-grade sodium sulfide, fully reacting for 1.5 hours under stirring at normal temperature, precipitating and separating 8003 grams of heavy metal-removed phosphoric acid liquid and 1.1 grams of filter residue, and using the filter residue separately;
and step B, adding 115 g of industrial-grade sodium hydroxide into 8003 g of the heavy metal-removed phosphoric acid solution obtained in the step A, fully reacting for 1.5 hours under normal temperature stirring, removing fluorine, filtering to separate 7865 g of the fluorine-removed phosphoric acid solution and filter residues, washing the filter residues with 200 g of water for several times until no acid smell exists, and drying to obtain 152 g of sodium fluosilicate products, wherein: na (Na) 2 SiF 6 The content is 98.10 percent, and washing water is added into the defluorinated phosphoric acid solution in the step to obtain 8073 g of defluorinated phosphoric acid solution; through the steps, fluorine in the wet-process phosphoric acid can be effectively recovered to form a sodium fluosilicate product, and meanwhile, the fluorine pollution to the environment caused by the fluorine contained in the phosphate fertilizer is avoided;
step C, adding 430 g of liquid ammonia into 8073 g of defluorinated phosphoric acid solution obtained in the step B at normal temperature until the pH value is 4.6, and carrying out neutralization exothermic reaction to preheat the slurry to obtain 8423 g of hot monoammonium phosphate slurry, so that the heat energy consumption during concentration is greatly reduced when the hot slurry is subjected to vacuum flash evaporation, and the purpose of saving heat energy is achieved;
d, performing vacuum flash evaporation on the hot monoammonium phosphate slurry obtained in the step C according to a conventional method, and evaporating water in the reaction slurry to obtain 7200 g of monoammonium phosphate slurry with the water content of 48.0%;
e, adding 1390 g of light-burned magnesia powder into 7200 g of the monoammonium phosphate slurry obtained in the step D, wherein the MgO content is 73.30%, carrying out neutralization exothermic reaction to obtain an ammonium magnesium phosphate semi-finished product, evaporating water in the reaction slurry, and further achieving the purpose of saving energy consumption;
step F, obtaining the product obtained in the step EStanding and curing the semi-finished product of magnesium ammonium phosphate for 30 days, curing the semi-finished product of magnesium ammonium phosphate into loose blocks, and conventionally crushing the loose blocks to obtain 7005 g of magnesium ammonium phosphate slow-release fertilizer, wherein: available phosphorus P 2 O 5 24.64%, mgO 18.21%, N5.31%. In the step, a large amount of free water is converted into solid crystal water in the curing process of magnesium ammonium phosphate ingeniously, and a drying process in the later period is omitted, so that the process is simplified, and energy conservation and consumption reduction are further realized.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (5)
1. The method for producing the magnesium ammonium phosphate slow-release fertilizer by using the wet-process phosphoric acid is characterized by comprising the following steps of:
A. adding sodium sulfide into low-concentration wet-process phosphoric acid according to the mass ratio of 0.05-0.1%, stirring and reacting for 60-100 minutes at normal temperature, removing heavy metals, settling or filtering to obtain phosphoric acid liquid without heavy metals and filter residues, and using the filter residues for another purpose; the wet process phosphoric acid is P 2 O 5 Wet process phosphoric acid with mass concentration of 15-25%;
B. adding sodium carbonate or sodium hydroxide into the phosphoric acid solution for removing heavy metals according to the molar ratio of Na to F =1:2-3 in wet-process phosphoric acid, reacting for 60-100 minutes under normal temperature stirring, defluorinating, filtering to obtain defluorinated phosphoric acid solution and filter residue, washing the filter residue until no acid smell exists, and drying to obtain a sodium fluosilicate product, wherein: na (Na) 2 SiF 6 The content is 98.10 percent, and washing water is merged into the defluorinated phosphoric acid solution;
C. adding liquid ammonia into the defluorinated phosphoric acid solution at normal temperature until the pH value is 4.5-5.0, and carrying out neutralization exothermic reaction to preheat the slurry to obtain hot monoammonium phosphate slurry;
D. carrying out vacuum flash evaporation on the hot monoammonium phosphate slurry, and evaporating water in the reaction slurry to obtain monoammonium phosphate slurry with the water content of less than 50%;
E. adding magnesium oxide powder into the monoammonium phosphate slurry according to the molar ratio of water-soluble phosphorus to MgO of 1:1-1.4, and performing neutralization exothermic reaction to obtain an ammonium magnesium phosphate semi-finished product;
F. and standing and curing the semi-finished product of magnesium ammonium phosphate, curing the semi-finished product of magnesium ammonium phosphate into loose blocks, and crushing or granulating the loose blocks to obtain the magnesium ammonium phosphate slow release fertilizer.
2. The method for producing magnesium ammonium phosphate slow-release fertilizer by using wet-process phosphoric acid as claimed in claim 1, wherein the sodium sulfide added in the step A, the sodium carbonate or sodium hydroxide added in the step B and the liquid ammonia added in the step C are all industrial-grade products.
3. The method for producing the magnesium ammonium phosphate slow-release fertilizer by the wet process phosphoric acid according to claim 1, wherein the magnesium oxide powder added in the step E is light-burned magnesium oxide powder with the magnesium oxide content of more than 60 percent.
4. The method for producing the magnesium ammonium phosphate slow-release fertilizer by the wet process phosphoric acid according to claim 1, wherein the curing time in the F is 15-30 days.
5. The method for producing magnesium ammonium phosphate slow-release fertilizer by using wet-process phosphoric acid as claimed in claim 1, wherein in the step D, the hot monoammonium phosphate slurry is subjected to vacuum flash evaporation to obtain monoammonium phosphate slurry with water content of 48% or less.
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| CN202210996544.2A CN115385319A (en) | 2020-09-07 | 2020-09-07 | Method for producing magnesium ammonium phosphate slow-release fertilizer by wet-process phosphoric acid |
| CN202010930650.1A CN112174699A (en) | 2020-09-07 | 2020-09-07 | Method for producing magnesium ammonium phosphate slow-release fertilizer by wet-process phosphoric acid |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1799996A (en) * | 2005-12-30 | 2006-07-12 | 云南省化工研究院 | Wet method phosphoric acid purification method |
| CN102020256A (en) * | 2010-11-22 | 2011-04-20 | 马健 | Method for producing industrial and agricultural monoammonium phosphate and magnesium ammonium phosphate with wet-process phosphoric acid |
| CN103936489A (en) * | 2014-04-29 | 2014-07-23 | 昆明隆祥化工有限公司 | Method for producing magnesium ammonium phosphate controlled-release fertilizer |
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| CN101456759B (en) * | 2008-11-28 | 2010-08-18 | 湖北兴发化工集团股份有限公司 | Method for producing magnesium ammonium phosphate composite fertilizer |
| CN105293459B (en) * | 2014-06-04 | 2017-08-18 | 深圳市芭田生态工程股份有限公司 | The method of the complete water-soluble MAP of Wet-process Phosphoric Acid Production and coproduction ammonium magnesium phosphate |
| CN104058378B (en) * | 2014-07-09 | 2015-11-18 | 昆明隆祥化工有限公司 | The method of monoammonium phosphate and magnesium ammonium phosphate is produced with the acid of wet method concentrated phosphoric acid slag |
| CN104261900A (en) * | 2014-09-01 | 2015-01-07 | 云南云天化国际化工有限公司 | Method for producing magnesium ammonium phosphate fertilizer by utilizing phosphoric acid sludge through wet process |
| CN110697674B (en) * | 2019-12-03 | 2021-03-30 | 中化重庆涪陵化工有限公司 | Method for producing magnesium ammonium phosphate by using high-magnesium phosphate tailings |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1799996A (en) * | 2005-12-30 | 2006-07-12 | 云南省化工研究院 | Wet method phosphoric acid purification method |
| CN102020256A (en) * | 2010-11-22 | 2011-04-20 | 马健 | Method for producing industrial and agricultural monoammonium phosphate and magnesium ammonium phosphate with wet-process phosphoric acid |
| CN103936489A (en) * | 2014-04-29 | 2014-07-23 | 昆明隆祥化工有限公司 | Method for producing magnesium ammonium phosphate controlled-release fertilizer |
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