Chemistry: fertilizers – Processes and products – Inorganic material
Reexamination Certificate
1999-07-21
2001-06-05
Langel, Wayne (Department: 1754)
Chemistry: fertilizers
Processes and products
Inorganic material
C071S034000, C423S308000, C423S310000
Reexamination Certificate
active
06241796
ABSTRACT:
This application is related to the application entitled “Method for Producing Fertilizer Grade DAP Having an Increased Nitrogen Concentration In a Spray Column”, filed concurrently herewith.
BACKGROUND OF THE INVENTION
1. Field of the Invention
The invention relates to a method of enhancing the nitrogen concentration of fertilizer grade DAP. Fertilizer grade DAP is defined in Official Publication No. 52 (1999) of the Association of American Plant Food Control Officials as a product composed of ammonium phosphates, principally diammonium phosphate, resulting from the ammoniation of phosphoric acid. It may contain up to 2 percent non-ammoniacal nitrogen. The guaranteed percentage of nitrogen and available phosphate shall be stated as part of the name.
2. Background of the Invention
Phosphorus as well as nitrogen are essential plant nutrients. Phosphorus and nitrogen ensure cell multiplication and thus growth since both are structural components of nucleic acids. Plants use the phosphorus and nitrogen to grow. Since fertilizers are generally formed by the reaction of phosphoric acid and ammonia, they are used to provide a rich source of nitrogen and phosphorus to the plants. Such fertilizers are generally applied to the soil and are readily assimilable by plants.
The phosphoric acid used in fertilizers is usually manufactured from rock phosphate typically in one of two ways. Phosphate rock is composed chiefly of calcium phosphates and calcite.
In the first prior art method, commonly known as the furnace acid process, the phosphoric acid is made by heating phosphate rock to a form of relatively pure elemental phosphorus which is then converted into the phosphoric acid. More particularly, this prior art process uses an electric furnace heated to about 1500° K. The phosphate rock is reduced by coke in the presence of sand or silicon dioxide according to the following reaction:
Ca
3
(PO
4
)
2
+3SiO
2
+5C═3CaSiO
3
+5CO+P
2
Gaseous P
2
condenses to form a solid P
4
. In the air, the P
4
converts to phosphorus pentoxide. Water is then added to the phosphorus pentoxide to form the phosphoric acid. The process usually yields 85 percent phosphoric acid which is colorless and has a density of about 1.69 kg/L. The phosphoric acid formed by this prior art process generally yields a purer phosphoric acid as compared to the phosphoric acid formed by the second prior art process, which is described below. However, this first process is also much more costly than the second prior art process.
The second prior art method used to produce phosphoric acid is known as the wet process. Most of the phosphoric acid produced in the United States is produced by this process. In this wet process, finely ground phosphate rock is slurried with sulfuric acid. Sometimes, recycled dilute phosphoric acid is included in the slurry. The reaction that occurs in this wet process is set forth below:
Ca
3
(PO
4
)
2
+3H
2
SO
4
=3CaSO
4
+2H
3
PO
4
In addition to the orthophosphoric acid, the reaction yields gypsum and numerous other suspended and dissolved impurities. The slurry is generally filtered to remove the solid impurities, mainly, gypsum. The resultant filtrate contains between 25 and 35 percent P
2
O
5
and between 1 and 8 percent by weight of suspended solids or impurities that are not removed by the filtration process. Examples of wet process methods are disclosed in U.S. Pat. Nos. 4,487,750, 4,485,078, 4,657,559, 4,665,790 and 4,655,789, which are incorporated herein in their entirety. U.S. Pat. No. 4,710,366 discloses methods of removing further impurities from the filtrate; such patent is incorporated herein in its entirety.
As used herein, the terms phosphoric acid and wet process phosphoric acid mean orthophosphoric acid.
Phosphoric acid is reacted with anhydrous ammonia to form ammonium phosphates, which constitute a large class of phosphorus fertilizers. See Examples 7 and 9 of U.S. Pat. No. 4,485,078. The common ammonium phosphates include monoammonium phosphate and diammonium phosphate, which are the primary components of the fertilizers commonly known as MAP and DAP, respectively. DAP (fertilizer grade) is a product composed of ammonium phosphates, principally diammonium phosphate, resulting from the ammoniation of phosphoric acid. The phosphoric acid is preferably reacted with the proper proportion of anhydrous ammonia which primarily provides diammonium phosphate, which is a source of nitrogen and phosphorus readily assimilable by food crops.
The TVA (Tennessee Valley Authority) in the early 1960s developed a process for the preparation of granular DAP from ammonia and phosphoric acid. The conventional TVA process for preparing granular DAP is described on pages 248 to 251 of
Manual of Fertilizer Processing
, edited by Francis T. Nielsson, Marcel Dekker, Inc., (1987). The conventional TVA type of process has a preneutralizer for partial ammoniation of the phosphoric acid and completion of ammoniation is done in a rotary ammoniator-granulator. Granulation is controlled by recycling product fines to the drum. The basic TVA process involves partial preneutralization of the acid in a preneutralizer (reaction tank) followed by completion of ammoniation to DAP in the rotary ammoniator-granulator. Excess ammonia, which must be fed to the ammoniator-granulator to produce DAP, is recovered by scrubbing the off gases with the acid to be used in the process. The granular product is normally dried, cooled, and screened, having the undersized and crushed oversized granular DAP recycled to the granulator to control granulation.
Pure diammonium phosphate [(NH
4
)
2
HPO
4
] is also termed dibasic ammonium phosphate. Page 561 of
The Merck Index,
10
th Ed., (1983), states that diammonium phosphate gradually loses about 8 percent NH
3
on exposure to air.
Triammonium phosphate is (NH
4
)
3
PO
4
.
BROAD DESCRIPTION OF THE INVENTION
An object of the invention is to provide a process for enhancing the ammoniacal nitrogen concentration of DAP. Another object of the invention is to provide a process for producing DAP fertilizer with the nitrogen and phosphate concentrations required for international trade, using the lower quality orthophosphoric acid currently being produced, without using expensive nitrogen supplements. A further object of the invention is to provide a process for the production of fertilizer grade diammonium phosphate. Other objects and advantages of the invention are set forth herein or are obvious herefrom to one skilled in the art.
The objects and advantages of the invention are achieved by the process of the invention.
There currently exists a need for a process to produce ammonium phosphate from orthophosphoric acid having a high concentration of impurities. Furthermore, a need exists for increasing the nitrogen content of DAP used for fertilizers. The invention provides a solution to such needs.
It has been found that reacting finely divided DAP with high pressure, anhydrous, gaseous ammonia will enhance or increase the ammoniacal nitrogen concentration of the DAP, but such treated DAP has the disadvantages that, as it ages, it tends to lose significant amounts of the added nitrogen and to gain excessive moisture.
The invention involves a process for enhancing the ammoniacal nitrogen concentration of DAP. The DAP, which is in finely divided form, is subjected to anhydrous gaseous ammonia, which is at a super atmospheric pressure and which is at a temperature sufficient to maintain the ammonia in the gaseous state. The increase in the ammoniacal nitrogen concentration is a function of the absolute ammonia pressure, the initial moisture content of the DAP and the contact time of the ammonia with the DAP. The enhancement of the ammoniacal nitrogen content of the DAP is also a function of the particle size of the DAP.
The DAP should be de-aerated before it is treated with the gaseous ammonia. The ammonia may have converted some of the DAP to triammonium phosphate and/or been adsorbed by the DAP.
A preferred embodiment of the invention proce
Astley Vaughn V.
Jardine Kenneth J.
Fisher Christen & Sabol
IMC-Agrico Company
Langel Wayne
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