CN117049929A - Method for producing spherical calcium ammonium nitrate particles by high tower granulation - Google Patents

Method for producing spherical calcium ammonium nitrate particles by high tower granulation Download PDF

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Publication number
CN117049929A
CN117049929A CN202311158937.7A CN202311158937A CN117049929A CN 117049929 A CN117049929 A CN 117049929A CN 202311158937 A CN202311158937 A CN 202311158937A CN 117049929 A CN117049929 A CN 117049929A
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China
Prior art keywords
calcium
magnesium
nitrate
ammonium nitrate
ammonium
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CN202311158937.7A
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Chinese (zh)
Inventor
崔瑞波
李腾飞
张梓榆
吕聪
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Shanxi Huaxin Fertilizer Corp
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Shanxi Huaxin Fertilizer Corp
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Priority to CN202311158937.7A priority Critical patent/CN117049929A/en
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    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05GMIXTURES 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
    • C05G5/00Fertilisers characterised by their form
    • C05G5/10Solid or semi-solid fertilisers, e.g. powders
    • C05G5/12Granules or flakes
    • CCHEMISTRY; METALLURGY
    • C05FERTILISERS; MANUFACTURE THEREOF
    • C05CNITROGENOUS FERTILISERS
    • C05C1/00Ammonium nitrate fertilisers

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Fertilizers (AREA)

Abstract

The application relates to the technical field of calcium ammonium nitrate, in particular to a method for producing spherical calcium ammonium nitrate particles by high-tower granulation. The application discloses a method for producing spherical calcium ammonium nitrate particles by high-tower granulation, which comprises the steps of proportioning and mixing, conveying a calcium ammonium nitrate mixed material containing trace magnesium into a primary mixing tank at the top of a granulating tower, and carrying out melt mixing with a calcium ammonium nitrate return material; after the melt mixing is finished, overflowing the mixture into a secondary mixing tank, and performing melt mixing again to obtain molten feed liquid; granulating, screening, namely enabling the molten feed liquid to enter a granulator through overflow for granulating, and cooling and screening to obtain an ammonium calcium nitrate product. Compared with the traditional granulating mode of the spraying method, the method adopts the high-tower melting granulating mode of the 'melt method', has lower energy consumption and lower dust emission, ensures that the particles of the ammonium calcium nitrate product are round and smooth, has no abnormal particles, has the particle size of 2-4mm, and meets the requirements of simultaneous sowing of seed and fertilizer and large-scale mechanized sowing.

Description

Method for producing spherical calcium ammonium nitrate particles by high tower granulation
Technical Field
The application relates to the technical field of calcium ammonium nitrate, in particular to a method for producing spherical calcium ammonium nitrate particles by high-tower granulation.
Background
At present, granular calcium ammonium nitrate (5 Ca (NO) 3 ) 2 ·NH 4 NO 3 ·10H 2 O), basically adopting a granulating mode of spraying slurry on a disc, a roller fluidized bed and a fluidized bed; the granulating mode of the disc and the roller fluidized bed has higher energy consumption, larger dust is generated in the granulating process, and a dust recovery device with higher energy consumption is required to be configured for treatment, so that the production cost is high, the environmental protection pressure is high, and the market competitiveness is weak;
the surface of the particles granulated by adopting the spraying granulation mode is not round, the product is irregular, the machine sowing fertilizer holes are easy to be blocked, so that large-scale continuous fertilizer sowing cannot be carried out by using the machine sowing, the requirements of simultaneously sowing seed and fertilizer and mechanically planting plants on a large scale are not met, and the use of the ammonium nitrate calcium fertilizer is seriously influenced.
Therefore, there is a need for a method for producing spherical calcium ammonium nitrate granules by high tower granulation, which produces spherical calcium ammonium nitrate granules with round surfaces, so as to meet the current market demands.
Disclosure of Invention
In order to overcome the defects of the prior art, the application provides a method for producing spherical calcium ammonium nitrate particles by high-tower granulation, which adopts a 'melt method' high-tower melting granulation mode, and has lower energy consumption, lower dust emission, round particles of calcium ammonium nitrate products, no abnormal particles and 2-4mm of product particle size, and meets the requirement of seed and fertilizer simultaneous sowing and mechanical large-scale machine sowing compared with the traditional 'slurry spraying method' granulation mode.
The technical scheme adopted for solving the technical problems is as follows:
a method for producing spherical calcium ammonium nitrate granules by high tower granulation, which comprises the following steps:
s1, batching
Preparing a calcium ammonium nitrate mixture containing a trace amount of magnesium;
or preparing a magnesium-free ammonium calcium nitrate mixture;
s2, mixing
Delivering the ammonium calcium nitrate mixed material containing trace magnesium into a primary mixing tank at the top of a granulating tower, and carrying out melt mixing with the ammonium calcium nitrate returned material; after the melt mixing is finished, overflowing the mixture into a secondary mixing tank, and performing melt mixing again to obtain molten feed liquid;
or conveying the ammonium calcium nitrate mixed material without magnesium to a primary mixing tank at the top of the granulating tower, and carrying out melt mixing with magnesium nitrate or calcium magnesium nitrate; after the melting and mixing are finished, overflowing the mixture into a secondary mixing tank, and carrying out melting and mixing on the mixture and the ammonium nitrate calcium return material to obtain molten feed liquid;
s3, granulating and screening
And (3) feeding the molten feed liquid into a granulator for granulation through overflow, and cooling and screening to obtain an ammonium calcium nitrate product.
Further, the specific gravity of the calcium ammonium nitrate mixture containing trace magnesium is 1.82-1.83g/cm 3 The mass ratio of the elemental magnesium is 0.1-0.5%.
Further, in step S1, the process of preparing the calcium ammonium nitrate mixture containing a trace amount of magnesium includes: calcium magnesium clear solution obtained by acidolysis and filter pressing of dolomite and nitric acid or magnesium clear solution obtained by reaction of nitric acid and light burned magnesium oxide is added into calcium nitrate clear solution in proportion, and evaporated and concentrated by a triple effect evaporator to prepare simple substance magnesium with mass ratio of 0.1-0.5% and specific gravity of 1.82-1.83g/cm 3 Calcium ammonium nitrate mixture containing trace magnesium.
Further, in step S1, the specific gravity of the magnesium-free calcium ammonium nitrate mixture is 1.82-1.83g/cm 3
Further, in step S1, the process of preparing the magnesium-free calcium ammonium nitrate mixture is as follows:
limestone and nitric acid react in an acidolysis tank to obtain acidolysis solution; adjusting the pH of acidolysis solution to 5-6, then performing filter pressing through a filter press to obtain clear calcium nitrate solution, and adding ammonium nitrate solution into the clear calcium nitrate solution to obtain mixed clear solution;
evaporating and concentrating the mixed clear liquid by a three-effect evaporator to prepare the product with the specific gravity of 1.82-1.83g/cm 3 Is mixed with the magnesium-free calcium ammonium nitrate.
Further, in step S2, the secondary mixing tank temperature is controlled to 90 ℃.
In step S2, the calcium magnesium nitrate mixed material is conveyed into a primary mixing tank at the top of a granulating tower, and is subjected to melt mixing with magnesium nitrate or calcium magnesium nitrate, so as to obtain a melt mixed liquid with the weight content of magnesium of 0.1-0.5%.
Further, the temperature of the three-effect evaporator in evaporation concentration is 120-130 ℃.
Further, in the step S3, the temperature of the product of the granulation lower tower is about 65 ℃, the product is cooled by a vibrating fluidized bed, and then the product is sieved by a roller sieve, so that the calcium ammonium nitrate product with the particle size of 2-4mm is obtained.
The beneficial effects of the application are as follows:
1. the method of the application adds magnesium nitrate and finished calcium magnesium nitrate into the ammonium calcium nitrate melt, or adds calcium magnesium clear solution or magnesium clear solution into the ammonium calcium nitrate dilute solution, and adds the ammonium calcium nitrate (5 Ca (NO 3 ) 2 ·NH 4 NO 3 ·10H 2 The mass content of the simple substance magnesium in the O) product is controlled to be between 0.1 and 0.5 percent, and the granulated ammonium calcium nitrate granule product has higher round strength and difficult caking and pulverization when meeting the national standard NY/T2269-2020 for ammonium calcium nitrate for agriculture, and is suitable for large-scale mass production.
2. Compared with the traditional granulating mode of the spraying method, the method adopts the high-tower melting granulating mode of the 'melt method', has lower energy consumption and lower dust emission, ensures that the particles of the ammonium calcium nitrate product are round and smooth, has no abnormal particles, has the particle size of 2-4mm, and meets the requirements of simultaneous sowing of seed and fertilizer and large-scale mechanized sowing.
Drawings
The application will be further described with reference to the drawings and examples.
FIG. 1 is a process flow diagram of the method of the present application;
FIG. 2 is a schematic diagram of the calcium ammonium nitrate product prepared in example 1 or example 2 according to the present application
FIG. 3 is a diagram of a calcium ammonium nitrate product prepared by the slurry spraying granulation method (comparative example 1) of the present application;
FIG. 4 is a diagram of the calcium ammonium nitrate product of example 3 according to the present application.
Detailed Description
As used herein, "and/or" includes any and all combinations of one or more of the associated listed items. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
Unless defined otherwise, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.
The exemplary application described herein may suitably lack any one or more of the element limitations not specifically disclosed herein. Thus, the terms "comprising," "including," "containing," and the like are to be construed broadly and without limitation. In addition, the term expressions which have been employed herein are used as terms of description and not of limitation, and there is no intention in the use of such terms of description not including any equivalents of the features shown and described, but rather, in accordance with the claims, various modifications are possible within the scope of the application. Thus, while the application has been specifically disclosed by preferred embodiments and optional features, modification of the application disclosed herein may be resorted to by those skilled in the art, and such modifications and variations are considered to be within the scope of this application.
The raw materials or reagents used in the examples and comparative examples of the present application were purchased from mainstream commercial manufacturers, and were of analytically pure grade that could be conventionally obtained without any particular limitation, as long as they were capable of achieving the intended effects. The apparatus and devices such as the magnetic stirrer used in this example are purchased from major commercial manufacturers, and are not particularly limited as long as they can function as intended. No particular technique or condition is identified in this example, which is performed according to techniques or conditions described in the literature in this field or according to product specifications.
In order to provide spherical calcium ammonium nitrate granules, the application provides a method for producing spherical calcium ammonium nitrate granules by high tower granulation, which comprises the following steps:
s1, batching
Calcium magnesium clear solution after acidolysis and filter pressing of dolomite and nitric acid is added into calcium nitrate clear solution in proportion or magnesium nitrate clear solution after reaction of nitric acid and light burned magnesium oxide is directly added, and the mixture is evaporated and concentrated by a triple effect evaporator to prepare simple substance magnesium with the mass ratio of 0.1-0.5% and the specific gravity of 1.82-1.83g/cm 3 Calcium ammonium nitrate mixture containing trace magnesium;
s2, mixing
Conveying the ammonium calcium nitrate mixed material containing trace magnesium in the step S1 to a first-stage mixing tank at the top of a granulating tower, and carrying out melt mixing with the ammonium calcium nitrate returned material; after mixing and melting, overflowing the mixture into a secondary mixing tank, mixing again to obtain molten material liquid, and controlling the final granulating temperature by controlling the circulating water quantity in a coil pipe of the secondary mixing tank;
or conveying the ammonium calcium nitrate mixed material without magnesium into a primary mixing tank at the top of a granulating tower, further mixing and melting the ammonium calcium nitrate mixed material with magnesium nitrate hexahydrate or finished calcium magnesium nitrate and ammonium calcium nitrate returned material under finished product screening, and then overflowing the mixture into a secondary mixing tank to obtain molten material, and controlling the final granulating temperature by controlling the circulating water quantity in a coil pipe of the secondary mixing tank;
the process for preparing the magnesium-free ammonium calcium nitrate mixture comprises the following steps: limestone and nitric acid react in an acidolysis tank to obtain acidolysis solution; adjusting pH of acidolysis solution to 5-6, press-filtering with a press filter to obtain calcium nitrate clear solution, and adding ammonium nitrate solution into the calcium nitrate clear solution to obtain a mixtureCombining the clear liquid; evaporating and concentrating the mixed clear liquid by a three-effect evaporator to prepare the product with the specific gravity of 1.82-1.83g/cm 3 Is mixed with the magnesium-free calcium ammonium nitrate.
S3, granulating and screening
And (3) feeding the molten feed liquid into a granulator for granulation through overflow, and cooling and screening to obtain an ammonium calcium nitrate product.
The application will be further illustrated by the following examples, which are not intended to limit the scope of the application, in order to facilitate the understanding of those skilled in the art.
Example 1
A method for producing spherical calcium ammonium nitrate granules by high tower granulation, which comprises the following steps:
limestone and nitric acid with the mass concentration of 45% are adopted to react in an acidolysis tank, the PH of acidolysis solution is regulated to be between 5 and 6, then calcium nitrate clear liquid with the mass concentration of 45% is obtained after filter pressing by a filter press, dolomite and nitric acid are added into the calcium nitrate clear liquid in proportion to be used for acidolysis and filter pressing, calcium magnesium clear liquid or magnesium nitrate clear liquid after the reaction of nitric acid and light burned magnesium oxide is directly added, and then the mixture is evaporated and concentrated by a triple effect evaporator until the final specific gravity of the material is 1.82-1.83g/cm 3 The content of the simple substance magnesium is 0.1-0.5%, and the temperature is 120-130 ℃ of the calcium ammonium nitrate mixture containing trace magnesium;
the ammonium calcium nitrate mixed material containing trace magnesium is then conveyed to a first-stage mixing tank at the top of a granulating tower through a melting pump, is further mixed and melted with ammonium calcium nitrate return material under finished product screening, enters a second-stage mixing tank through overflow, and finally, the temperature of the second-stage mixing tank is controlled to be 90 ℃ by adopting an automatic regulating valve to control the circulating water quantity in a coil pipe of the second-stage mixing tank, and enters a differential granulator through overflow for granulation.
The temperature of the product of the granulation lower tower is about 65 ℃, the temperature is about 45 ℃ after the air cooling of the vibrating fluidized bed, and then the product is screened by a two-stage roller screen to be controlled to be the grain size2-4Between mm, the finished product is sent to a full-automatic packaging and stacking line through a bucket elevator, so that the round particles and full water solubility are obtained, and the requirements of the standard of agricultural ammonium calcium nitrate and use regulations of NY/T2269-2020 are metA product; the appearance and particle status of the product are shown in fig. 2.
Example 2
A method for producing spherical calcium ammonium nitrate granules by high tower granulation, which comprises the following steps:
limestone and nitric acid with the mass concentration of 45% are adopted to react in an acidolysis tank, the PH of acidolysis solution is regulated to be between 5 and 6, calcium nitrate clear solution with the mass concentration of 45% is obtained after filter pressing by a filter press, ammonium nitrate solution is added into the calcium nitrate clear solution according to a proportion, and the mixture is evaporated and concentrated by a triple effect evaporator until the specific gravity of the final material is 1.82-1.83g/cm 3 Magnesium-free calcium ammonium nitrate mixture at 120-130 ℃.
The ammonium calcium nitrate mixed material without magnesium is conveyed to a primary mixing tank at the top of a granulating tower through a melting pump, finished magnesium nitrate hexahydrate or finished calcium magnesium nitrate is added into a mixing tank, the content of elemental magnesium in the molten liquid is controlled to be between 0.1 and 0.5 percent, the magnesium nitrate hexahydrate or the finished calcium magnesium nitrate is further mixed with ammonium calcium nitrate return material under finished product screening to be melted, the mixture enters a secondary mixing tank through overflow, the circulating water quantity in a coil pipe of the secondary mixing tank is controlled through an automatic regulating valve, the temperature of the secondary mixing tank is controlled to be 90 ℃, and the mixture enters a differential granulator through overflow to be granulated.
The temperature of the product in the lower tower of granulation is about 65 ℃, the temperature is about 45 ℃ after being cooled by a vibrating fluidized bed, and then the product is sieved by a two-stage roller sieve, and the grain size is controlled to be the same2-4The finished product is sent to a full-automatic packaging and stacking line through a bucket elevator, so that the finished product is round and smooth in particles, and the full water solubility meets the standard requirements of agricultural calcium ammonium nitrate and use regulations of NY/T2269-2020. The appearance and particle status of the calcium ammonium nitrate product are shown in figure 2.
Example 3
A method for producing spherical calcium ammonium nitrate granules by high tower granulation, which comprises the following steps:
magnesium nitrate or calcium magnesium nitrate is not added into the ammonium calcium nitrate dilute solution or the melt to adjust the magnesium content in the ammonium calcium nitrate, other operation indexes and processes are consistent with those of the embodiment 1, and the obtained product has non-round particle appearance, 20N strength and easy caking and pulverization. The appearance and particle status of the calcium ammonium nitrate product are shown in fig. 4.
Example 4
A method for producing spherical calcium ammonium nitrate granules by high tower granulation, which comprises the following steps:
the other control modes are the same as those of the example 2, and when the granulating temperature is controlled to be more than 94 ℃, the granulated calcium ammonium nitrate is not formed, the sticking tower is serious, when the granulating temperature is controlled to be 91-94 ℃, the granules are more in special shape, the tower is easy to stick, and the optimal granulating temperature is 90 ℃.
Comparative example 1
A method of producing spherical calcium ammonium nitrate granules comprising the steps of:
the procedure of example 1 was followed using disk granulation, roller fluidized bed and fluidized bed slurry spray granulation. The appearance and particle status of the calcium ammonium nitrate product are shown in figure 3.
The calcium ammonium nitrate products prepared in examples 1 to 4 and comparative example 1 were tested according to the standard of agricultural calcium ammonium nitrate and use procedure of NY/T2269-2020, and the results are summarized in Table 1 below.
TABLE 1
The above embodiments are preferred embodiments of the present application, and besides, the present application may be implemented in other ways, and any obvious substitution is within the scope of the present application without departing from the concept of the present application.

Claims (9)

1. A method for producing spherical calcium ammonium nitrate granules by high tower granulation, which is characterized by comprising the following steps:
s1, batching
Preparing a calcium ammonium nitrate mixture containing a trace amount of magnesium;
or preparing a magnesium-free ammonium calcium nitrate mixture;
s2, mixing
Delivering the ammonium calcium nitrate mixed material containing trace magnesium into a primary mixing tank at the top of a granulating tower, and carrying out melt mixing with the ammonium calcium nitrate returned material; after the melt mixing is finished, overflowing the mixture into a secondary mixing tank, and performing melt mixing again to obtain molten feed liquid;
or conveying the ammonium calcium nitrate mixed material without magnesium to a primary mixing tank at the top of the granulating tower, and carrying out melt mixing with magnesium nitrate or calcium magnesium nitrate; after the melting and mixing are finished, overflowing the mixture into a secondary mixing tank, and carrying out melting and mixing on the mixture and the ammonium nitrate calcium return material to obtain molten feed liquid;
s3, granulating and screening
And (3) feeding the molten feed liquid into a granulator for granulation through overflow, and cooling and screening to obtain an ammonium calcium nitrate product.
2. The method according to claim 1, wherein in step S1, the specific gravity of the trace magnesium-containing calcium ammonium nitrate mixture is 1.82-1.83g/cm 3 The mass ratio of the elemental magnesium is 0.1-0.5%.
3. The method according to claim 1 or 2, characterized in that in step S1 the formulation of the calcium ammonium nitrate mix containing trace amounts of magnesium comprises: calcium magnesium clear solution obtained by acidolysis and filter pressing of dolomite and nitric acid or magnesium clear solution obtained by reaction of nitric acid and light burned magnesium oxide is added into calcium nitrate clear solution in proportion, and evaporated and concentrated by a triple effect evaporator to prepare simple substance magnesium with mass ratio of 0.1-0.5% and specific gravity of 1.82-1.83g/cm 3 Calcium ammonium nitrate mixture containing trace magnesium.
4. The method according to claim 1, wherein in step S1, the specific gravity of the magnesium-free calcium ammonium nitrate mixture is 1.82-1.83g/cm 3
5. The method according to claim 1 or 4, wherein in step S1, the process of formulating the magnesium-free calcium ammonium nitrate mix is:
limestone and nitric acid react in an acidolysis tank to obtain acidolysis solution; adjusting the pH of acidolysis solution to 5-6, then performing filter pressing through a filter press to obtain clear calcium nitrate solution, and adding ammonium nitrate solution into the clear calcium nitrate solution to obtain mixed clear solution;
evaporating and concentrating the mixed clear liquid by a three-effect evaporator to prepare the product with the specific gravity of 1.82-1.83g/cm 3 Is mixed with the magnesium-free calcium ammonium nitrate.
6. The method according to claim 1, wherein in step S2, the secondary mixing tank temperature is controlled to 90 ℃.
7. The method according to claim 1, wherein in step S2, the calcium magnesium nitrate mixture is fed to a primary mixing tank at the top of the granulation tower and melt-mixed with magnesium nitrate or calcium magnesium nitrate to obtain a melt-mixed liquid having a magnesium content of 0.1 to 0.5% by weight.
8. The method of claim 5, wherein the three-effect evaporator is at a temperature of 120-130 ℃.
9. The method according to claim 1, wherein in step S3, the granulated product is cooled at about 65 ℃ by a vibrating fluid bed and then sieved by a drum sieve to obtain a calcium ammonium nitrate product with a particle size of 2-4 mm.
CN202311158937.7A 2023-09-08 2023-09-08 Method for producing spherical calcium ammonium nitrate particles by high tower granulation Pending CN117049929A (en)

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CN202311158937.7A CN117049929A (en) 2023-09-08 2023-09-08 Method for producing spherical calcium ammonium nitrate particles by high tower granulation

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311158937.7A CN117049929A (en) 2023-09-08 2023-09-08 Method for producing spherical calcium ammonium nitrate particles by high tower granulation

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