Chemistry: fertilizers – Processes and products – Inorganic material
Reexamination Certificate
1998-07-21
2001-01-23
Griffin, Steven P. (Department: 1754)
Chemistry: fertilizers
Processes and products
Inorganic material
C071S054000, C071S058000, C071S059000, C071S061000, C071S064010, C071S064030, C071S064130, C023S3130FB, C023S3130FB
Reexamination Certificate
active
06176892
ABSTRACT:
This application is a 371 application of International application No. PCT/NO96/00244, filed Oct. 18, 1996.
The present invention relates to a method for preparation of nitrate and potassium containing fertilizers (NK-fertilizers) in particulated form. The invention further comprises products of such NK-fertilizers.
NK-fertilizers can be made by blending N-fertilizers with K-fertilizers, but there has been a need for having at least some homogeneous formulations of NK-fertilizers. The N-source can be urea or a nitrate fertilizer such as ammonium nitrate or calcium nitrate (CN) and the potassium source can be a K-fertilizer like KNO
3
(KN), KCI, or K
2
SO
4
. However, particulation, both with regard to prilling and granulation, has proved to cause great problems. Thus it has been experienced that when CN and KNO
3
have been melted together, substantial undercooling caused severe problems for the particulation step. A NK-fertilizer based on CN and KNO
3
was considered to be most interesting as it could be expected to possess all the advantages of a CN-fertilizer and in addition contain water-soluble potassium from a nitrate source.
From Japanese application JP 95005421 B2 it is known a granular NK-fertilizer made from an eutectic material consisting of 90-50 weight % urea and 10-50 weight % potash (potassium carbonate). The granular product is made by spraying through a small hole the eutectic solution on raw material which is fed into a kneader and then mixed and melted. For equalizing the elution speed of the nitrogen and the potash, the granules are covered with a coating material having polypropylene resin as a major component. This is a most complicated process. Such a fertilizer will have a large part of its nitrogen as NH
4
—N and corresponding loss of this nitrogen. The reason for this is of course that urea constitutes the only N-source of the fertilizer. Further, there will be no water-soluble calcium as will be the case when CN and KNO
3
are the N-sources.
Addition of a potassium source to a nitrogen-potassium fertilizer is known from U.S. Pat. No. 3,617,235 which comprises spraying melts or suspensions with a low water content and containing the plant nutrients nitrogen and phosphorous. Solid potassium salt is added before spraying or prilling said melt or suspension. However, this process requires that solids added are graded so that more than 7 weight % has a grain size exceeding 0.1 mm. Though this process functions excellently for NPK-fertilizer, this principle has not been found to be useful for particulating NK-fertilizers, mainly due to the undercooling problems and that the required particle size for the solids is not available in the market.
The main object of the invention was to arrive at a new method for particulating NK-melts or solutions into homogeneous NK-fertilizers.
Another object was to arrive at a method for making NK-fertilizers based on calcium nitrate fertilizers and potassium nitrate.
A further object was to develop a method for making NK-fertilizers which in addition also contained other nutrients like magnesium nitrate.
It was also an object to arrive at homogeneous NK-fertilizers which could be applied alone or as blending components either for special NK-formulations or NPK-fertilizer blends.
Due to the disadvantages related to known NK-fertilizers, it was decided to investigate further the possibilities of applying CN and KNO
3
as basic raw materials for the new fertilizer. Throughout this description the abbreviation CN is meant to cover both pure calcium nitrate and the calcium nitrate product obtained from a nitrophosphate process. This product is often called Norsk Hydro Calcium Nitrate abbreviated NH-CN and has the following composition: 79 weight % calcium nitrate, 6 weight % ammonium nitrate and 15 weight % water. Several ways of making the desired NK-fertilizer formulations were evaluated. Thus compactation of prilled CN and crystalline KNO
3
and blending of available prilled CN and prilled KNO
3
were tested. Compactation was found to be expensive and gave a product with rather high dust content. Blending is first of all dependent on having similar particles with regard to particle size and particle size distribution for the two raw materials in question. Secondly, a homogeneous product will not be obtained.
Though undercooling was considered to be a problem, the inventors decided to investigate further making homogeneous NK-fertilizer from melts of at least one of the components and possibly add the other component as solids to the melt. Solid KNO
3
was dissolved in melted CN, but initial tests showed that then the undercooling was so severe that prilling/granulation would be impossible. Series of experiments were conducted adding solid KNO
3
, having various particle size, to melted CN at about 100° C. The particle size of the solids was varied between 0.2-1.6 mm. The question was whether the mixture could solidify before the KNO
3
particles dissolved in the CN melt and thereby resulted in undercooling of the melt. During these experiments the ratios between CN and KNO
3
were also varied. The following two formulations were especially tested: 70 weight % CN and 30 weight % KNO
3
, corresponding to the NPK-formulation (defined as N—P
2
O
5
—K
2
O) 15-0-14, and 85 weight % CN and 15 weight % KNO
3
, corresponding to the formulation 15-0-7. However, during all these experiments some undercooling was experienced. If the particle size of the solids <0.3 mm, the undercooling was substantial. To avoid undercooling the particle size of the solids should be larger than 1 mm. But KNO
3
having this particle size is not available on the market and in addition such large particles would cause problems during prilling. Though it might be possible to obtain particulated homogeneous NK-fertilizers with this method, it was not considered to be the ultimate solution to the problem and further investigations of this method were terminated.
Then it was decided to perform a thorough investigation of the various phases for CN-water-KNO
3
. During these investigations it was surprisingly found that there was indeed an area where undercooling would not cause substantial problems. Accordingly, it should be possible to perform particulation by applying traditional methods and equipment. This area can be defined as follows:
Ca(NO
3
)
2
40-14 weight %
KNO
3
55-85 weight %
Water
0.5-6 weight %
It was further found that to such NK-melts/solutions MgNO
3
, could be added in amounts of 0-5 weight %. The fertilizer mixture to be particulated could also contain 0-4 weight % ammonium nitrate (AN).
In view of these findings particulation of melts/solutions within the above ranges was performed. Successful prilling could be carried out at temperatures of 160-190° C. and granulation could be conducted at temperatures of 90-140° C. Thus it was obtained homogeneous NK-fertilizer products having particle size of 1-5 mm and within desired size distribution. The products were of nice spherical shape and the particles had a hardness or crushing strength of about 2-13 kg, depending on water content and size.
The present invention thus provides a method for making NK-fertilizers which comprises melting calcium nitrate fertilizer and potassium nitrate at 90-120° C. to form a melt or suspension thereof, heating the melt or suspension to a temperature suitable for particulation, and particulating the heated melt or suspension to form a homogeneous NK-fertilizer.
Preferably the components are mixed in ratios giving a melt or suspension comprising 40-14 weight % calcium nitrate, 55-85 weight % potassium nitrate, 0.5-6 weight % water, 0-4 weight % ammonium nitrate and 0-5 weight % magnesium nitrate.
The particulation can be performed by prilling at temperatures of 160-190° C., or by granulation of a melt or suspension containing 10-2.5 weight % water at a granulation temperature of 90-140° C.,
For example, about 60 weight % potassium nitrate and about 40 weight % of a calcium nitrate fertilizer are melted at about 100° C. forming a melt containing about 60
Isaksen Jan Birger
Moland Lars Gustav
Obrestad Torstein
Griffin Steven P.
Nave Eileen E.
Norsk Hydro ASA
Wenderoth , Lind & Ponack, L.L.P.
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