CN114380632A - NP and NPK fertilizer containing polyphosphate and water-soluble calcium and preparation method thereof - Google Patents
NP and NPK fertilizer containing polyphosphate and water-soluble calcium and preparation method thereof Download PDFInfo
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- CN114380632A CN114380632A CN202011144029.9A CN202011144029A CN114380632A CN 114380632 A CN114380632 A CN 114380632A CN 202011144029 A CN202011144029 A CN 202011144029A CN 114380632 A CN114380632 A CN 114380632A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
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- 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
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Abstract
The invention discloses a preparation method of an NPK or NP material containing oligomeric phosphate and water-soluble calcium. The method controls the melt temperature and/or residence time and/or feeding sequence to ensure that the obtained material contains oligomeric phosphate, water-soluble calcium and N/P in NPK material2O5The ratio of N to P2O5The ratio of (A) to (B) is 3.0. gtoreq.N/P2O5≥1.0，P2O5The ratio of Ca/17.8 > P2O5The ratio of/Ca is more than 6.8, and the ratio of N to P in NP material2O5The ratio of 2.2 > N/P2O5＞1.2，P2O5The ratio of Ca/Ca is 24.5 > P2O5the/Ca is more than 9.0. 95% of phosphorus element contained in the NP and NPK fertilizers exists in a form of water-soluble phosphorus compounds, and 98% of calcium element exists in a form of water-soluble calcium compounds. The NP fertilizer and the NPK fertilizer of the present invention contain water-soluble calcium and water-soluble phosphorus, and the water-soluble phosphorus moietyThe fertilizer has the advantages of existence of condensed phosphate forms, high content of soluble phosphorus and water-soluble calcium, quick and long-acting fertilizer effect.
Description
Technical Field
The invention relates to the technical field of compound fertilizers, in particular to NPK and NP fertilizers containing polyphosphate and water-soluble calcium and a preparation method thereof.
Background
The water-soluble phosphate in the fertilizer is very easily fixed by metal cations such as iron and aluminum in the soil, so that the utilization rate of phosphorus in the fertilizer is low, and the fertilizer cannot move in the soil. The prior art is directed to changing a single orthophosphate radical into a phosphate radical which is dimeric or trimeric, so as to improve the effectiveness of phosphorus in soil, and a recognized technical path is that a single orthophosphate can be polymerized according to a reaction formula (1):
n(H3PO4) + Heat → Hn+2PnO3n+1+nH2O、、、、(1)
The polymerization degree n used in general agriculture is between 2 and 7, the water solubility is good, and the crop absorption rate is high; when n is more than or equal to 30, the ammonium polyphosphate is in the category of industrial ammonium polyphosphate, has no water solubility, and is mainly used for fire extinguishing materials. The common method for preparing the oligomeric phosphate is to polymerize phosphoric acid at high temperature by a wet method and add a condensing agent (ammonia, urea, dicyandiamide, melamine, ammonium sulfate and the like) at the same time; the second is thermal method using phosphorus pentoxide as starting material, and the third is by heating hydrogen phosphate. However, the existing preparation method has some problems.
The method is the most common method at present, and most manufacturers adopt the method to produce the agricultural ammonium polyphosphate. As disclosed in the present application, a method for preparing iron phosphate and ammonium polyphosphate fertilizers from phosphated slag generated from zinc-manganese or zinc-based phosphated metal surfaces, the process comprises: adding 85% phosphoric acid and urea according to a certain proportion, and carrying out sectional heating condensation at 110 ℃ and 120 ℃ to prepare the ammonium polyphosphate fertilizer. In another method disclosed so far, a novel method for producing an aqueous solution of ammonium polyphosphate with low degree of polymerization by a low-temperature method was created, which comprises the following steps: the method is characterized in that polyphosphoric acid with the concentration of 100-120% is used as a main raw material, and ammonium bicarbonate is added to adjust the polyphosphoric acid to produce low-polymerization-degree ammonium polyphosphate aqueous solution with the nitrogen content of more than 11% and the phosphorus pentoxide content of more than 37% in batch, wherein dimer (ammonium pyrophosphate) is used as a main raw material.
Urea or ammonium bicarbonate is mentioned as a condensing agent in the two cases, but polyphosphoric acid in the second case is polyphosphoric acid per se, the meaning of polymerizing and synthesizing the polyphosphoric acid by monophosphorous radicals is not reflected, and the first case can not be directly applied to the preparation of compound fertilizer melt granulation.
In addition, calcium in the compound fertilizer is also very easy to be fixed by orthophosphate radical and sulfate radical, which causes that the calcium of the fertilizer is not water-soluble, the effectiveness is poor and the absorption of crops is difficult. The existing compound fertilizers are designed to physically separate calcium from phosphate radical and sulfate radical, and a set of compound fertilizers without calcium and calcium fertilizers are adopted for matching, or EDTA-Ca and other chelated calcium are added in reciprocating compound fertilizers, but the cost is higher. For example, in the currently disclosed calcium-containing compound fertilizer, plant peptides are prepared by multi-bacteria fermentation, and calcium powder is prepared after the plant peptides are chelated with calcium compounds, and is mixed with macroelement raw materials for granulation. However, the currently disclosed calcium-containing compound fertilizer does not mention how much the chelation rate of calcium and peptide can be achieved, and cannot be applied to the preparation of compound fertilizer melt granulation.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides an NP fertilizer, an NPK fertilizer and a preparation method of the NP fertilizer and the NPK fertilizer, so as to solve the technical problem that the existing compound fertilizer does not contain water-soluble calcium or does not contain water-soluble polyphosphate by carrying out complexing treatment or melt granulation on the calcium.
In order to achieve the above object, according to one aspect of the present invention, there is provided an NP fertilizer. The NP fertilizer comprises nitrogen element, phosphorus element and calcium element, wherein the phosphorus element is P2O5The weight ratio of the calcium element, the nitrogen element and the phosphorus element in the NP fertilizer is 24.5 & gt P2O5/Ca＞9.0，2.2＞N/P2O5＞1.2；
Wherein the phosphorus element is at least partially water-solublePhosphorus compound, the calcium element is at least partially in the form of water-soluble calcium compound, and P is2O5The water-soluble phosphorus element accounts for at least 95 wt% of the total amount of available phosphorus, and the water-soluble calcium accounts for at least 98 wt% of the total amount of available calcium;
the water-soluble phosphorus compound comprises condensed phosphate, with P2O5The condensed phosphate accounts for at least 8 wt% of the total weight of the NP fertilizer.
In one aspect of the invention, a method for preparing an NP fertilizer is provided. The preparation method of the NP fertilizer comprises the following steps:
melting the nitrogen compound in a dissolving tank to form a molten nitrogen compound;
adding a phosphate radical-containing compound into the molten nitrogen compound, and carrying out heat preservation melting treatment at 145-170 ℃ for 40-60 minutes to form a molten mixture;
introducing the molten mixture into a mixing tank, and adding a calcium compound into the molten mixture for reaction;
wherein the nitrogen compound, the phosphate-containing compound and the calcium compound are in a weight ratio of (40-45): (8-24): (5-8) performing material adding treatment.
In yet another aspect of the present invention, an NPK fertilizer is provided. The NPK fertilizer contains nitrogen element, phosphorus element and potassium element, and also contains calcium element, wherein the phosphorus element is P2O5The weight ratio of the calcium element, the nitrogen element and the phosphorus element in the NPK fertilizer is 17.8 & gt P2O5/Ca＞6.8，3.0≥N/P2O5≥1.0；
Wherein the phosphorus element is at least partially present in the form of a water-soluble phosphorus compound, the calcium element is at least partially present in the form of a water-soluble calcium compound, and P is2O5The water-soluble phosphorus element accounts for at least 95 wt% of the total amount of available phosphorus, and the water-soluble calcium accounts for at least 98 wt% of the total amount of available calcium;
the water-soluble phosphorus compound comprises condensed phosphate, with P2O5The condensed phosphate accounts for at least NP fertilizer2 wt% of the total amount of the material.
In another aspect of the invention, a method for preparing an NPK fertilizer is provided. The preparation method of the NPK fertilizer comprises the following steps:
melting the nitrogen compound in a dissolving tank to form a molten nitrogen compound;
adding a phosphate radical-containing compound into the molten nitrogen compound, and carrying out heat preservation melting treatment at 145-170 ℃ for 40-60 minutes to form a molten mixture;
introducing the molten mixture into a mixing tank, adding a calcium compound into the molten mixture for reaction, and then adding a potassium compound;
wherein the nitrogen compound, the phosphate group-containing compound, the calcium compound and the potassium compound are (40-45) in weight ratio: (8-24): (5-8): (30-40) performing material adding treatment.
Compared with the prior art, the NP fertilizer and the NPK fertilizer contain water-soluble calcium and water-soluble phosphorus, the water-soluble phosphorus part exists in a condensed phosphate form, the soluble phosphorus and the water-soluble calcium are high in content, and the absorption of plants is facilitated, for example, the water-soluble phosphorus accounts for more than 95 wt% of the total amount of available phosphorus, the water-soluble calcium accounts for more than 98 wt% of the total amount of available calcium, wherein the content of the condensed phosphate in the NP fertilizer is more than 8 wt%, and the content of the condensed phosphate in the NPK fertilizer is more than 2 wt%. In addition, the nitrogen, phosphorus, potassium and calcium elements have proper content proportion, meet the requirements of plants on nutrient elements and are beneficial to the growth of the plants.
The preparation method of the NP fertilizer and the NPK fertilizer adopts a melt granulation process, and the corresponding compounds are subjected to a melting reaction for preparation, so that the prepared NP fertilizer and the prepared NPK fertilizer contain water-soluble calcium and water-soluble phosphorus, the water-soluble phosphorus exists in a condensed phosphate form, and the fertilizer effect is quick-acting and long-acting.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic process flow diagram of a preparation method of an NP fertilizer according to an embodiment of the present invention;
FIG. 2 is a schematic process flow diagram of a preparation method of the NPK fertilizer according to the embodiment of the invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the present application, "at least one" means one or more, "a plurality" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (a), b, and c", may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, and c may be single or plural, respectively.
It should be understood that, in various embodiments of the present application, the sequence numbers of the above-mentioned processes do not mean the execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weight of the related components mentioned in the description of the embodiments of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present application as long as it is scaled up or down according to the description of the embodiments of the present application. Specifically, the mass in the description of the embodiments of the present application may be in units of mass known in the chemical industry, such as μ g, mg, g, and kg.
In one aspect, embodiments of the present invention provide an NP fertilizer. The NP fertilizer contains a calcium element in addition to a nitrogen element and a phosphorus element which is P2O5The weight ratio of the calcium element, the nitrogen element and the phosphorus element in the NP fertilizer is 24.5 & gt P2O5/Ca＞9.0，2.2＞N/P2O5＞1.2。
Wherein, the phosphorus element contained in the NP fertilizer of the embodiment of the invention is at least partially in the form of water-soluble phosphorus compound, and is measured as P2O5The water-soluble phosphorus element accounts for at least 95 wt% of the total available phosphorus in the NP fertilizer of the embodiment of the invention. It was further determined that the water-soluble phosphorus compound included a condensed phosphate salt, as P2O5The condensed phosphate accounts for at least 8 wt% of the total weight of the NP fertilizer. Therefore, the content of the phosphorus element contained in the NP fertilizer has a proper proportion to the content of the nitrogen element, the content of the soluble phosphorus element is high, and the absorption of plants to the phosphorus element is improved.
Since the condensed phosphate is soluble phosphorus, the condensed phosphate is obtained by condensationThe phosphate-bonded salts are oligomeric phosphates. In one embodiment, P is2O5The condensed phosphate is at least 8 wt% of the total NP fertilizer, and in further embodiments, the condensed phosphate is at least 8-25 wt% of the total NP fertilizer. In a specific embodiment, the degree of polymerization of the condensed phosphate is 2 to 7. Wherein the condensed phosphate can be metaphosphate, pyrophosphate, hexametaphosphate and the like. The condensed phosphate has high content in the NP fertilizer in the embodiment of the invention and is oligomeric phosphate, so the condensed phosphate has good water solubility and improves the absorption effect of plants on phosphorus elements.
The calcium element contained in the NP fertilizer of the embodiment of the invention is at least partially in the form of a water-soluble calcium compound, and the water-soluble calcium element is determined to be at least 98 wt% of the total amount of effective calcium in the NP fertilizer of the embodiment of the invention. Therefore, the NP fertilizer contains calcium in a proper proportion to nitrogen and phosphorus, and is high in soluble calcium content, so that the absorption of plants to the calcium is improved. In a specific embodiment, the water-soluble calcium element may be Ca (PO)3)2Exist in the form of (1).
Therefore, the NP fertilizer of the embodiment of the invention contains high content of water-soluble calcium and water-soluble phosphorus, and the water-soluble phosphorus part exists in a condensed phosphate form, thereby being beneficial to the absorption of plants. In addition, the content proportion of nitrogen, phosphorus and calcium elements is proper, the requirement of plants on nutrient elements is met, and the growth of the plants is facilitated.
Based on the NP fertilizer, the embodiment of the invention also provides a preparation method of the NP fertilizer. The preparation method of the NP fertilizer has the process flow as shown in figure 1, and comprises the following steps:
s01: melting the nitrogen compound in a dissolving tank to form a molten nitrogen compound;
s02: adding a phosphate radical-containing compound into the molten nitrogen compound, and carrying out heat preservation melting treatment at 145-170 ℃ for 40-60 minutes to form a molten mixture;
s03: introducing the molten mixture into a mixing tank, and adding a calcium compound into the molten mixture for reaction.
Thus, the preparation method of the NP fertilizer provided by the embodiment of the invention adopts a melt granulation process to prepare the corresponding compound through a melt reaction, so that the prepared NP fertilizer contains water-soluble calcium and water-soluble phosphorus, the water-soluble phosphorus exists in a condensed phosphate form, and the water-soluble calcium, the water-soluble phosphorus and the condensed phosphate are high in content.
In step S01, the nitrogen compound melting process may be performed according to a nitrogen compound melting temperature. In this embodiment, the temperature of the melt processing is 145 ℃ to 175 ℃ for 50 minutes to 70 minutes. This temperature is effective to melt the nitrogen compound, and also facilitates the melt processing of the phosphate group-containing compound in step S02.
In addition, the nitrogen compound is a nitrogen providing element, and therefore, in one embodiment, the nitrogen compound preferably comprises ammonium phosphorus nitrate, but may be other nitrogen fertilizer raw materials commonly used in high towers. In a specific embodiment, the ammonium phosphate nitrate comprises at least one of 32-4-0 ammonium phosphate nitrate and 33-4.5-0 ammonium phosphate nitrate. Wherein the water-soluble phosphorus in the 32-4-0 ammonium nitrate phosphorus and/or the 33-4.5-0 ammonium nitrate phosphorus accounts for more than or equal to 99 percent of available phosphorus.
When the nitrogen compound is ammonium phosphorus nitrate, the ammonium phosphorus nitrate is subjected to a reaction represented by the following reaction formula (2) during the melt processing:
NH4NO3→NH3+HNO3+ absorbing heat ", (2)
The ammonium phosphorus nitrate containing higher free acid can react with the following reaction formula (3) in the longer time of melting treatment:
NH4NO3→N2O+HNO3+ release of heat ", (3)
The heat released by the reaction of reaction formula (3) is accumulated in the molten mass without heat exchange, in preparation for the reaction of the phosphate group-containing compound in step S02.
Next, the step S01 may be performed in a dissolving tank, and specifically, the nitrogen compound is placed in the dissolving tank of the NP fertilizer preparation process and heated for melting.
In step S02, after the phosphate-containing compound is added to the molten nitrogen compound in step S01, a polymerization reaction shown in the following reaction formula (4) occurs under the effect of high temperature, and at least part of the condensed phosphate is generated:
n(H2PO- 4) + heat → (PO)- 3)n+nH2O、、、、(4)
Further, the phosphate-containing compound is a compound which supplies phosphorus element and also supplies phosphate to at least partially undergo polymerization at high temperature to produce the condensed phosphate as described above, specifically, as shown in the reaction formula (4), and the phosphorus-containing nitrogen compound is melt-reacted with the phosphate compound to produce oligomeric Phosphate (PO)-3)n. To ultimately produce the NP fertilizer described above. Therefore, the phosphate-containing compound is prepared by mixing the nitrogen compound, the phosphate-containing compound and the calcium compound in a weight ratio of (66-75): (10-26): (5-8) performing material adding treatment. The N/P in the finally generated NP fertilizer is controlled by controlling the addition amount of the phosphate radical-containing compound2O5The ratio is 2.2 > N/P2O5＞1.2。
In one embodiment, the temperature of the soaking and melting treatment in the step S02 is 145-175 ℃, preferably 145-170 ℃ for 40-60 minutes. The polymerization reaction in the reaction formula (4) is controlled by controlling the temperature and time of the heat-insulating melting treatment, so that the content of the soluble condensed phosphate in the finally generated NP fertilizer is adjusted and optimized, and the content of the soluble phosphorus is increased.
In one embodiment, the phosphate-containing compound preferably comprises ammonium dihydrogen phosphate, although other phosphate source materials commonly used in high towers are also possible. In a specific embodiment, the ammonium dihydrogen phosphate comprises at least one of ammonium dihydrogen phosphate 12-60-0 and ammonium dihydrogen phosphate 12-61-0. Wherein the water-soluble phosphorus in the 12-60-0 ammonium dihydrogen phosphate and/or the 12-61-0 ammonium dihydrogen phosphate accounts for more than or equal to 99 percent of the available phosphorus. The phosphate radical-containing compound contains phosphate radical and can be subjected to polymerization reaction in molten state, specifically, the phosphate radical compound such as ammonium nitrate phosphorus and the like is molten with the nitrogen compound such as ammonium dihydrogen phosphate and the likeMelting reaction to generate oligomeric Phosphate (PO)-3)nThereby increasing the content of water-soluble phosphorus.
Next, the step S02 may be performed in the dissolution tank, and specifically, the melting treatment may be performed in the dissolution tank of the NP fertilizer preparation process.
In the step S03, after the calcium compound is added to the molten mixture in the step S02, the reaction shown in the following reaction formula (5) is performed under the effect of high temperature, and the soluble calcium compound, specifically calcium metaphosphate (Ca (PO) (calcium metaphosphate) which is a soluble calcium compound, is at least partially generated3)2) At the same time, the reaction is accelerated to the direction of oligomeric phosphate, and a certain amount of free acid is kept and a certain amount of water is evaporated, so that Ca (PO) can be allowed3)2In the presence of acid or water vapor, the fertilizer is rapidly decomposed into calcium dihydrogen phosphate and changed into water-soluble calcium (6), so that NP and NPK fertilizers containing oligophosphates and water-soluble calcium are prepared:
Ca2++(PO- 3)2→Ca(PO3)2、、、、(5)
Ca(PO- 3)2+2H2O→Ca(H2PO4)2、、、、(6)
in addition, the calcium compound provides calcium element. In order to finally produce the above NP fertilizer, therefore, the calcium compound is in a weight ratio of (66-75): (10-26): (5-8) performing material adding treatment. The P in the finally generated NP fertilizer is controlled by controlling the adding amount of the calcium compound2O5The ratio of/Ca is 24.5 > P2O5/Ca＞9.0。
In one embodiment, the temperature of the calcium compound reaction in step S03 may be the temperature of the heat-insulated melting treatment in S02, such as 145 ℃ to 175 ℃, preferably 145 ℃ to 170 ℃, for 40 to 60 minutes. The content of the soluble calcium in the finally generated NP fertilizer is adjusted and optimized by controlling the temperature and the time of the reaction of the calcium compound so as to control the generation amount of the soluble calcium in the reaction formula (5), thereby improving the content of the soluble calcium.
In one embodiment, the calcium compound comprises at least one of calcium ammonium nitrate, calcium magnesium nitrate liquid. The calcium-containing compound can generate soluble calcium in a molten state according to the double decomposition combination reaction of oligomeric phosphate radicals, so that the content of the water-soluble calcium is increased.
Next, the step S03 may be performed in a primary tank, specifically, in a primary tank of the NP fertilizer preparation process, performing heat preservation melting treatment.
After step S03, a back-end cooling granulation is also included. In a specific embodiment, the back-end cooling granulation comprises a high tower air cooling, planar water cooling granulation process.
Therefore, the preparation method of the NP fertilizer in each of the above embodiments adopts a melt granulation process to prepare the corresponding compound by melt reaction, so that the prepared NP fertilizer contains water-soluble calcium and water-soluble phosphorus, and the water-soluble phosphorus exists in a condensed phosphate form, and the water-soluble calcium, the water-soluble phosphorus and the condensed phosphate are high in content. And the content of each element and the content of water-soluble calcium and oligomeric phosphate of the generated NP fertilizer can be optimized and improved by controlling the process conditions of each step. In addition, the preparation method of the NP fertilizer provided by the embodiment of the invention has the advantages that the process flow is simple and easy to control, the prepared NP fertilizer has stable fertilizer efficiency, and the industrialization is easy to realize.
On the other hand, the embodiment of the invention also provides an NPK fertilizer. The NPK fertilizer contains a calcium element in addition to a nitrogen element, a phosphorus element and a potassium element, wherein the phosphorus element is P2O5The weight ratio of the calcium element, the nitrogen element and the phosphorus element in the NPK fertilizer is 17.8 & gt P2O5/Ca＞6.8，3.0≥N/P2O5≥1.0。
Wherein, the NPK fertilizer of the embodiment of the invention at least partially exists in the form of water-soluble phosphorus compound, and is measured to be P2O5The water-soluble phosphorus element accounts for at least 95 wt% of the total available phosphorus in the NPK fertilizer of the embodiment of the invention. It was further determined that the water-soluble phosphorus compound included a condensed phosphate salt, as P2O5Said condensed phosphate is at leastAccounting for 2wt percent of the total weight of the NPK fertilizer. Therefore, the NPK fertilizer contains phosphorus and nitrogen in proper proportion, and has high soluble phosphorus content, so that the absorption of plants to the phosphorus is improved.
Since the condensed phosphate is soluble phosphorus, the condensed phosphate is an oligomeric phosphate. In one embodiment, P is2O5The condensed phosphate is at least 2 wt% of the total amount of NPK fertilizer, and in further embodiments, the condensed phosphate is at least 2-15 wt% of the total amount of NPK fertilizer. In a specific embodiment, the degree of polymerization of the condensed phosphate is 2 to 7. Wherein the condensed phosphate can be metaphosphate, pyrophosphate, hexametaphosphate and the like. The condensed phosphate has high content in the NPK fertilizer in the embodiment of the invention and is oligomeric phosphate, so the condensed phosphate has good water solubility and improves the absorption effect of plants on phosphorus elements.
The NPK fertilizer of the embodiment of the invention at least partially contains calcium which exists in the form of water-soluble calcium compound, and the water-soluble calcium is determined to be at least 98 wt% of the total amount of effective calcium in the NPK fertilizer of the embodiment of the invention. Therefore, the NPK fertilizer contains calcium element in a proper proportion to nitrogen element and phosphorus element, and has high soluble calcium content, thereby improving the absorption of plants to the calcium element. In a specific embodiment, the water-soluble calcium element may be Ca (PO)3)2Exist in the form of (1).
In addition, the K content in the NPK fertilizer of each of the above examples may be a content conventionally used for NPK fertilizers.
Therefore, the NPK fertilizer of the embodiment of the invention contains high content of water-soluble calcium and water-soluble phosphorus, and the water-soluble phosphorus part exists in a condensed phosphate form, thereby being beneficial to the absorption of plants. In addition, the nitrogen, phosphorus, potassium and calcium elements have proper content proportion, meet the requirements of plants on nutrient elements and are beneficial to the growth of the plants.
Based on the NPK fertilizer, the embodiment of the invention also provides a preparation method of the NPK fertilizer. The preparation method of the NPK fertilizer has the process flow as shown in figure 2, and comprises the following steps:
s04: melting the nitrogen compound in a dissolving tank to form a molten nitrogen compound;
s05: adding a phosphate radical-containing compound into the molten nitrogen compound, and carrying out heat preservation melting treatment at 145-170 ℃ for 40-60 minutes to form a molten mixture;
s06: introducing the molten mixture into a mixing tank, adding a calcium compound into the molten mixture for reaction, and adding a potassium compound into the molten mixture.
Thus, the preparation method of the NPK fertilizer provided by the embodiment of the invention adopts a melt granulation process to carry out a melt reaction on the corresponding compound for preparation, so that the prepared NPK fertilizer contains water-soluble calcium and water-soluble phosphorus, the water-soluble phosphorus exists in a condensed phosphate form, and the water-soluble calcium, the water-soluble phosphorus and the condensed phosphate are high in content.
Here, the step S04 may be performed with full reference to the step S01 of the above NP fertilizer preparation method, and thus, when the nitrogen compound is ammonium phosphorus nitrate, the nitrogen compound is melted to react as shown in the above reaction formulas (2) and (3) during the melting process in the step S04, and the product is the same as the product generated during the melting process in the step S01. Since the step S04 can be performed with full reference to the step S01 of the NP fertilizer preparation method, the step S04 will not be described herein for the sake of brevity.
The step S05 may be performed with full reference to the step S02 of the NP fertilizer preparation method described above, so that, during the heat-retaining melting treatment in the step S05, the phosphate-containing compound undergoes the reaction shown in the reaction formula (4) described above, and the same product is produced as that produced during the melting treatment in the step S02, and the phosphorus-containing nitrogen compound and the phosphate compound undergo a melting reaction to produce an oligomeric Phosphate (PO)-3)nSpecifically, a nitrogen compound such as ammonium nitrate phosphorus and the like is subjected to a melt reaction with a phosphate compound such as ammonium dihydrogen phosphate and the like to produce an oligomeric Phosphate (PO)-3)n. Since the step S05 can be performed with full reference to the step S02 of the NP fertilizer preparation method, the step S05 will not be described herein for the sake of brevity.
In addition, the phosphate-containing compound in step S05 is prepared by mixing the nitrogen compound, the phosphate-containing compound, the calcium compound and the potassium compound in a weight ratio of (40-45): (8-24): (5-8): (30-40) performing material adding treatment.
The preliminary calcium compound addition reaction to the molten mixture in the step S06 may be performed completely with reference to the above step S03 of the NP fertilizer manufacturing method, and thus, during the calcium compound addition reaction in the step S06, the calcium compound reacts as shown in the above reaction formula (5) and the product is the same as the product generated during the melting process in the step S03. Since the step of adding calcium compound in step S06 can be performed with full reference to step S03 of the NP fertilizer preparation method, in step S06, the reactions shown in the following reaction formulas (5) and (6) also occur at high temperature, and at least part of the soluble calcium compound, specifically, calcium metaphosphate (Ca (PO) is generated3)2) At the same time, the reaction is accelerated to the direction of oligomeric phosphate, and a certain amount of free acid is kept and a certain amount of water is evaporated, so that Ca (PO) can be allowed3)2In the presence of acid or water vapor, the calcium phosphate is rapidly decomposed into calcium dihydrogen phosphate and becomes water-soluble calcium, so as to achieve the preparation of NP and NPK fertilizers containing oligophosphates and water-soluble calcium, and for saving space, the step of adding calcium compound in the step S06 for reaction is not repeated.
The potassium compound is added in step S06 to add potassium element to the molten mixture. In one embodiment, the potassium compound preferably comprises potassium sulfate, but may be other potassium fertilizer materials commonly used in high towers. The potassium compound can be effectively dispersed in the molten mixture without affecting the contents of the water-soluble calcium and the water-soluble phosphorus generated by the reactions in the steps S04 to S06.
In addition, the calcium compound and the potassium compound are mixed according to the weight ratio of the nitrogen compound, the phosphate group-containing compound, the calcium compound and the potassium compound being (40-45): (8-24): (5-8): (30-40) performing material adding treatment.
Secondly, the step of adding the potassium compound may be performed in a secondary tank, in particular a mixing process in a secondary tank of a process for preparing NPK fertilizers.
After step S06, a back-end cooling granulation is also included. In a specific embodiment, the back-end cooling granulation comprises a high tower air cooling, planar water cooling granulation process.
Therefore, the NPK fertilizer preparation method in each of the above embodiments adopts a melt granulation process to prepare the corresponding compound by melt reaction, so that the prepared NPK fertilizer contains water-soluble calcium and water-soluble phosphorus, and the water-soluble phosphorus exists in the form of condensed phosphate, and the water-soluble calcium, the water-soluble phosphorus and the condensed phosphate are high in content. And the content of each element of the generated NPK fertilizer and the content of water-soluble calcium and oligomeric phosphate can be optimized and improved by controlling the process conditions of each step. In addition, the preparation method of the NPK fertilizer provided by the embodiment of the invention has the advantages that the process flow is simple and easy to control, the prepared NPK fertilizer has stable fertilizer efficiency, and the industrialization is easy to realize.
The present invention will now be described in further detail with reference to specific NP and NPK fertilizers and methods for their preparation as examples.
NP fertilizer and method for producing the same
Example 11
The present example provides an NP fertilizer and a method for preparing the same. The NP fertilizer contains 46% of formula 28-13-0 (containing Ca 1.44%) and N/P2O5The ratio of (A) to (B) is 2.15, P2O5The ratio of/Ca was 9.03 and contained water-soluble calcium and water-soluble phosphorus as shown in Table 1.
The preparation method of the NP fertilizer comprises the following steps:
s1: putting the ammonium phosphate nitrate (33-4.5-0, 76 wt%) in a dissolving tank, keeping the temperature at 160 +/-15 ℃, keeping the retention time for 60 +/-10 minutes, and carrying out melting treatment to form a molten nitrogen compound;
s2: keeping the temperature of the molten nitrogen compound unchanged in the step S1, adding ammonium dihydrogen phosphate (12-60-0, 16 wt%) into the molten nitrogen compound in the step S1, and keeping the residence time for 50 minutes +/-10 minutes for heat preservation and melting treatment to form a molten mixture;
s3: discharging the molten mixture in the step S2 into a primary tank, adding calcium ammonium nitrate (8 wt%) for reaction, and sending the molten mixture to a rear end cooling granulation treatment after the reaction is finished.
Example 12
The present example provides an NP fertilizer and a method for preparing the same. The NP fertilizer has a content of 44% and a formula of 27-17-0 (containing Ca 0.9%), and N/P2O5The ratio of (A) to (B) is 1.59, P2O5The ratio of/Ca was 18.89, and contained water-soluble calcium and water-soluble phosphorus as shown in Table 1.
The preparation method of the NP fertilizer comprises the following steps:
s1: putting the ammonium phosphate nitrate (33-4.5-0, 72 wt%) in a dissolving tank, keeping the temperature at 160 +/-15 ℃, keeping the retention time for 60 +/-10 minutes, and carrying out melting treatment to form a molten nitrogen compound;
s2: keeping the temperature of the molten nitrogen compound unchanged in the step S1, adding ammonium dihydrogen phosphate (12-60-0, 23 wt%) into the molten nitrogen compound in the step S1, and keeping the residence time for 50 minutes +/-10 minutes for heat preservation and melting treatment to form a molten mixture;
s3: discharging the molten mixture in the step S2 into a primary tank, adding calcium ammonium nitrate (5 wt%) for reaction, and sending the molten mixture into a rear end cooling granulation treatment after the reaction is finished.
Example 13
The present example provides an NP fertilizer and a method for preparing the same. The NP fertilizer contains 47% of formula 25-22-0 (containing Ca 0.9%), and N/P2O5The ratio of (A) to (B) is 1.14, P2O5The ratio of/Ca was 24.44, and the water-soluble calcium and the water-soluble phosphorus were contained as shown in Table 1.
The preparation method of the NP fertilizer comprises the following steps:
s1: putting the ammonium phosphate nitrate (33-4.5-0, 63 wt%) in a dissolving tank, keeping the temperature at 160 +/-15 ℃, keeping the retention time for 60 +/-10 minutes, and carrying out melting treatment to form a molten nitrogen compound;
s2: keeping the temperature of the molten nitrogen compound unchanged in the step S1, adding ammonium dihydrogen phosphate (12-60-0, 32 wt%) into the molten nitrogen compound in the step S1, and keeping the residence time for 50 minutes +/-10 minutes for heat preservation and melting treatment to form a molten mixture;
s3: discharging the molten mixture in the step S2 into a primary tank, adding calcium ammonium nitrate (5 wt%) for reaction, and sending the molten mixture into a rear end cooling granulation treatment after the reaction is finished.
The NP fertilizers of examples 11 to 13 were subjected to the following ingredient tests in table 1, respectively, and the test results are shown in table 1:
TABLE 1 NP assay results
NPK fertilizer and preparation method thereof
Example 21
The present example provides an NPK fertilizer and a method of preparing the same. The NPK fertilizer contains 46% of formula 21-21-7 (containing Ca 1.44%) and N/P2O5The ratio of 1 to P2O5The ratio of Ca/water soluble calcium and phosphorus was 15 and shown in Table 2.
The preparation method of the NPK fertilizer comprises the following steps:
s1: putting the ammonium phosphate nitrate (33-4.5-0, 49 wt%) in a dissolving tank, keeping the temperature at 160 +/-15 ℃, keeping the retention time for 60 +/-10 minutes, and carrying out melting treatment to form a molten nitrogen compound;
s2: keeping the temperature of the molten nitrogen compound unchanged in the step S1, adding ammonium dihydrogen phosphate (12-60-0, 32 wt%) into the molten nitrogen compound in the step S1, and keeping the residence time for 50 minutes +/-10 minutes for heat preservation and melting treatment to form a molten mixture;
s3: discharging the molten mixture in the step S2 into a primary tank, and adding calcium ammonium nitrate (8 wt%) for reaction;
s4: discharging the molten mixture obtained in the step S3 into a secondary tank, adding potassium mannheim sulfate (0-0-52, 11 wt%), uniformly mixing, and sending to the rear end for cooling and granulating.
Example 22
The present example provides an NPK fertilizer and a method of preparing the same. The NPK fertilizer content is 48% of formula 16-16-16 (containing Ca 0).9%) and N/P2O5The ratio of 1 to P2O5The ratio of/Ca was 17.78, and the water-soluble calcium and the water-soluble phosphorus were contained as shown in Table 2.
The preparation method of the NPK fertilizer comprises the following steps:
s1: putting the ammonium phosphate nitrate (33-4.5-0, 41 wt%) in a dissolving tank, keeping the temperature at 160 +/-15 ℃, keeping the retention time for 60 +/-10 minutes, and carrying out melting treatment to form a molten nitrogen compound;
s2: keeping the temperature of the molten nitrogen compound unchanged in the step S1, adding ammonium dihydrogen phosphate (12-60-0, 24 wt%) into the molten nitrogen compound in the step S1, and keeping the residence time for 50 minutes +/-10 minutes for heat preservation and melting treatment to form a molten mixture;
s3: discharging the molten mixture obtained in the step S2 into a primary tank, and adding calcium ammonium nitrate (5 wt%) for reaction;
s4: discharging the molten mixture obtained in the step S3 into a secondary tank, adding potassium mannheim sulfate (0-0-52, 30 wt%), uniformly mixing, and sending to the rear end for cooling and granulating.
Example 23
The present example provides an NPK fertilizer and a method of preparing the same. The NPK fertilizer has a content of 44% in formula 18-6-20 (containing Ca 0.9%), and N/P2O5The ratio of (A) to (B) is 3, P2O5The ratio of/Ca was 6.67 and contained water-soluble calcium and water-soluble phosphorus as shown in Table 2.
The preparation method of the NPK fertilizer comprises the following steps:
s1: putting the ammonium phosphate nitrate (33-4.5-0, 50.5 wt%) in a dissolving tank, keeping the temperature at 160 +/-15 ℃, keeping the retention time for 60 +/-10 minutes, and carrying out melting treatment to form a molten nitrogen compound;
s2: keeping the temperature of the molten nitrogen compound unchanged in the step S1, adding ammonium dihydrogen phosphate (12-60-0, 6.5 wt%) into the molten nitrogen compound in the step S1, and keeping the residence time for 50 minutes +/-10 minutes for heat preservation and melting treatment to form a molten mixture;
s3: discharging the molten mixture obtained in the step S2 into a primary tank, and adding calcium ammonium nitrate (5 wt%) for reaction;
s4: discharging the molten mixture obtained in the step S3 into a secondary tank, adding potassium mannheim sulfate (0-0-52, 38 wt%), uniformly mixing, and sending to the rear end for cooling and granulating.
The NPK fertilizers of examples 21 to 23 were subjected to the following ingredient tests in table 2, respectively, and the test results are shown in table 2:
TABLE 2 NPK test results
As can be seen from the content tests of the relevant components in tables 1 and 2, the NP fertilizer and the NPK fertilizer of the examples of the invention contain high content of water-soluble calcium and water-soluble phosphorus, and the water-soluble phosphorus part exists in the form of condensed phosphate, which is beneficial to the absorption of plants. In addition, the nitrogen, phosphorus, potassium and calcium elements have proper content proportion, meet the requirements of plants on nutrient elements and are beneficial to the growth of the plants.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The NP fertilizer comprises nitrogen element and phosphorus element, and is characterized by further comprising calcium element, wherein the phosphorus element is P2O5The weight ratio of the calcium element, the nitrogen element and the phosphorus element in the NP fertilizer is 24.5 & gt P2O5/Ca＞9.0，2.2＞N/P2O5＞1.2；
Wherein the phosphorus element is at least partially present in the form of a water-soluble phosphorus compound, the calcium element is at least partially present in the form of a water-soluble calcium compound, and P is2O5The water-soluble phosphorus element accounts for at least 95 wt% of the total amount of available phosphorus, and the water-soluble calcium element accounts for at least 98 wt% of the total amount of available calcium;
the water-soluble phosphorus compound comprises condensed phosphate, with P2O5The condensed phosphate accounts for at least 8 wt% of the total weight of the NP fertilizer.
2. The NP fertilizer material of claim 1, wherein: the condensed phosphate at least accounts for 8-25 wt% of the total weight of the NP fertilizer; and/or
The polymerization degree of the condensed phosphate is 2-7.
3. The preparation method of the NP fertilizer is characterized by comprising the following steps:
melting the nitrogen compound in a dissolving tank to form a molten nitrogen compound;
adding a phosphate radical-containing compound into the molten nitrogen compound, and carrying out heat preservation melting treatment at 145-170 ℃ for 40-60 minutes to form a molten mixture;
introducing the molten mixture into a mixing tank, and adding a calcium compound into the molten mixture for reaction;
wherein the nitrogen compound, the phosphorus compound and the calcium compound are (66-75) in weight ratio: (10-26): (5-8) performing material adding treatment.
4. The production method according to claim 3, characterized in that: and introducing the molten mixture into the mixing tank when the water content of the molten mixture is less than or equal to 1.0 wt%.
5. The production method according to claim 3 or 4, characterized in that: the nitrogen compound comprises at least one of 32-4-0 ammonium phosphate nitrate and 33-4.5-0 ammonium phosphate nitrate; and/or
The phosphate radical-containing compound comprises at least one of ammonium dihydrogen phosphate 12-60-0 and ammonium dihydrogen phosphate 12-61-0; and/or
The calcium compound comprises at least one of calcium ammonium nitrate, calcium nitrate and calcium magnesium nitrate liquid.
6. The NPK fertilizer comprises nitrogen element, phosphorus element and potassium element, and is characterized by further comprising calcium element, wherein the phosphorus element is P2O5The weight ratio of the calcium element, the nitrogen element and the phosphorus element in the NPK fertilizer is 17.8 & gt P2O5/Ca＞6.8，3.0≥N/P2O5≥1.0；
Wherein the phosphorus element is at least partially present in the form of a water-soluble phosphorus compound, the calcium element is at least partially present in the form of a water-soluble calcium compound, and P is2O5The water-soluble phosphorus element accounts for at least 95 wt% of the total amount of available phosphorus, and the water-soluble calcium element accounts for at least 98 wt% of the total amount of available calcium;
the water-soluble phosphorus compound comprises condensed phosphate, with P2O5The condensed phosphate accounts for at least 2 wt% of the total weight of the NPK fertilizer.
7. The NPK fertilizer of claim 6, wherein: the condensed phosphate at least accounts for 2-15 wt% of the total amount of the NPK fertilizer; and/or
The polymerization degree of the condensed phosphate is 2-7.
8. The preparation method of the NPK fertilizer is characterized by comprising the following steps:
melting the nitrogen compound in a dissolving tank to form a molten nitrogen compound;
adding a phosphate radical-containing compound into the molten nitrogen compound, and carrying out heat preservation melting treatment at 145-170 ℃ for 40-60 minutes to form a molten mixture;
introducing the molten mixture into a mixing tank, adding a calcium compound into the molten mixture for reaction, and then adding a potassium compound;
wherein the nitrogen compound, the phosphate group-containing compound, the calcium compound and the potassium compound are (40-45) in weight ratio: (8-24): (5-8): (30-40) performing material adding treatment.
9. The method of claim 8, wherein: and introducing the molten mixture into the mixing tank when the water content of the molten mixture is less than or equal to 1.0 wt%.
10. The production method according to claim 8 or 9, characterized in that: the nitrogen compound comprises at least one of 32-4-0 ammonium phosphate nitrate and 33-4.5-0 ammonium phosphate nitrate, and the water-soluble phosphorus in the 32-4-0 ammonium phosphate nitrate and/or the 33-4.5-0 ammonium phosphate nitrate accounts for more than or equal to 99 percent of the available phosphorus; and/or
The phosphate radical-containing compound comprises at least one of 12-60-0 ammonium dihydrogen phosphate and 12-61-0 ammonium dihydrogen phosphate, and the phosphorus occupying the water soluble phosphorus in the 12-60-0 ammonium dihydrogen phosphate and/or the 12-61-0 ammonium dihydrogen phosphate is more than or equal to 99%; and/or
The calcium compound comprises at least one of calcium ammonium nitrate, calcium nitrate and calcium magnesium nitrate liquid; and/or
The potassium compound comprises at least one of potassium sulfate and potassium chloride.
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