JP2017132659A - Granular nitrogen fertilizer, and method for producing the granular nitrogen fertilizer - Google Patents
Granular nitrogen fertilizer, and method for producing the granular nitrogen fertilizer Download PDFInfo
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本発明は、粒硬度が高いため粉体発生量が少なく、保管中の固結性の低い粒状窒素肥料およびその製造方法に関するものである。 TECHNICAL FIELD The present invention relates to a granular nitrogen fertilizer having a low particle generation amount due to high grain hardness and a low caking property during storage, and a method for producing the same.
窒素肥料の一つである硫安は、工業的にはコークス炉廃ガスを硫酸と接触させることや、カプロラクタムの生成過程において、カプロラクタム硫酸塩にアンモニアを添加して得られる硫安水溶液を晶析することで得られる。肥料として求められる硫安の物理的性質は、「機械施肥に支障がないこと」「粒径２〜４ｍｍに大部分が収まること」「粒径２．０〜２．８ｍｍのものについての圧壊強度の平均が２ｋｇｆ以上」「水分１．０％以下」「安息角４０°以下」「製品の固結等理化学的品質に悪影響をおよぼさないこと」とされている（非特許文献１）。 Ammonium sulphate, one of the nitrogen fertilizers, industrially contacts coke oven waste gas with sulfuric acid, and crystallizes the aqueous ammonium sulfate solution obtained by adding ammonia to caprolactam sulfate during the process of caprolactam formation. It is obtained by. The physical properties of ammonium sulfate required as a fertilizer are “no hindrance to mechanical fertilization”, “mainly within a particle size of 2 to 4 mm”, “crushing strength of a particle size of 2.0 to 2.8 mm” The average is 2 kgf or more, “moisture of 1.0% or less”, “rest angle of 40 ° or less”, and “not to adversely affect physicochemical quality such as consolidation of products” (Non-patent Document 1).
窒素肥料の硫安粉状品および細粒品は、粒が小さく舞いやすいため、機械散布時の発塵や、流路つまりが生じやすく、肥料として必須用件である「機械施肥に支障がないこと」には適さない。散布時の発塵が少なく、流路のつまりが生じづらいことは、機械散布が主流である広大な農地での施肥において重要である。そこで、これら課題を克服すべく硫安の粉状品および細粒品を粉状窒素肥料として造粒し、粒径を２〜４ｍｍ程度に粒径を大きくすることで粒径が大きいため、圧壊強度が高く、流動性が良好な肥料とすることが検討されている（特許文献１〜５）。 Nitrogen fertilizer ammonium sulphate powder and fine-grained products tend to be small and flakes easily, so dust generation and flow path clogging are likely to occur during machine spraying, which is an essential requirement for fertilizers. Is not suitable. It is important for fertilization in vast agricultural land where mechanical spraying is the mainstream that dust generation during spraying is small and that clogging of the flow path is difficult to occur. Therefore, in order to overcome these problems, powdered and fine granules of ammonium sulfate are granulated as powdered nitrogen fertilizer, and the particle size is increased by increasing the particle size to about 2 to 4 mm. Therefore, it has been studied to make a fertilizer having high fluidity and good fluidity (Patent Documents 1 to 5).
例えば、バリが少なく、圧壊強度が高く、窒素濃度が高く、固結しづらいといった肥料に適した物理的特性を持つ造粒窒素の肥料の造粒方法を提供するために、窒素肥料を圧縮造粒する際の、ポケットサイズ、造粒圧力、バリ厚みを制御することで窒素肥料を造粒する方法（特許文献１）や、硫安結晶を中間サイズ、小さいサイズ、大きいサイズに分離し、中間サイズを肥料に適したサイズとして単離後、小さいサイズ、大きいサイズからなる残留結晶を原料として粒状肥料に造粒する方法（特許文献２）が提案されている。 For example, in order to provide a granulation method for granulated nitrogen fertilizer with physical properties suitable for fertilizers such as few burrs, high crushing strength, high nitrogen concentration, and difficult to consolidate, nitrogen fertilizer is compressed and formed. Method of granulating nitrogen fertilizer by controlling pocket size, granulation pressure, burr thickness when granulating (Patent Document 1), and separating ammonium sulfate crystals into intermediate size, small size, large size, intermediate size Has been proposed (Patent Document 2) of granulating a granular fertilizer using residual crystals of small size and large size as a raw material after isolation as a size suitable for fertilizer.
また粒状窒素肥料の製造においては、肥料として取り扱う際に、造粒した硫安が粉状になる「粉化」や、長期間保管した際に製造した造粒硫安同士が固まる「固結」が発生すると、機械散布時の作業性を悪化させてしまう。そのため、粉化や固結を抑制する方法が検討されている。例えば、粉化については、造粒後に分級して得られた微粒硫安を原料硫安と混合してコンパクタに投入することで、角張った形状の微粒硫安と丸い形状の硫安が混合することで、圧縮されて強く固まり、保管 ・取り扱い中に崩壊しにくい造粒方法（特許文献３）が提案されている。固結については、粒状硫安を造粒するにあたり、硫安の一部にワックスや界面活性剤などの固結防止剤を添加してから、残りの硫安を混合して圧縮造粒する方法（特許文献４）や、粒状窒素肥料にトレハロースなど糖類を溶質とする溶液を混合することで被覆し、水分の吸収及び放出を抑制して固結防止する方法（特許文献５）がある。 In the production of granular nitrogen fertilizer, when handling as fertilizer, the pulverized ammonium sulfate is pulverized, and when the granulated ammonium sulfate is solidified when stored for a long period of time, "solidification" occurs. Then, workability at the time of machine spraying is deteriorated. Therefore, methods for suppressing pulverization and consolidation have been studied. For example, with regard to pulverization, by mixing fine ammonium sulfate obtained by classification after granulation with raw material ammonium sulfate and introducing it into a compactor, the angular shaped fine ammonium sulfate and round-shaped ammonium sulfate are mixed. A granulation method (Patent Document 3) has been proposed in which it is strongly solidified and stored and hardly disintegrates during handling. For granulation, when granulating granular ammonium sulfate, add anti-caking agent such as wax or surfactant to a part of ammonium sulfate, then mix the remaining ammonium sulfate and compress granulate (Patent Document) 4) and a method in which granular nitrogenous fertilizer is coated by mixing a solution containing a saccharide such as trehalose as a solute, thereby suppressing absorption and release of moisture (Patent Document 5).
前記の通り、様々な粒状窒素肥料やその製造方法が提案されており、粒状窒素肥料の長期保管中に問題となる固結についてはその防止対策として固結防止材の添加を行うなど実施しているが、十分な効果が得られていない。また、固結防止材の添加は追加工程が必要なためコストが高くなる。特許文献１では、粒状品であれば、粒径が大きいため圧壊強度が高く、比表面積が低いため、水分が低く固結が発生しづらいと記載されているが、圧壊強度が高く、比表面積が低ければ、必ずしも水分が低いわけではなく、水分が多ければ粒径が大きくても固結が発生する。特許文献２では、結晶の粒径を選択して造粒しているが、中間サイズを造粒せずに単離することが目的であり、固結防止に対する効果はない。また物理的特性に影響を及ぼす添加剤の使用について特許文献２に記載があるが、固結防止材を加えるとしても追加工程や追加コストが必要である。特許文献３では、造粒後に分級して得られた微粒硫安を原料硫安と混合して造粒することで崩壊しにくい硫安とすることが記載されているが、微粒硫安のリサイクルは一般的に実施されている内容であるのに加えて、固結防止に対する効果は記載がなく、また特許文献１と同様に水分が高ければ固結が発生する。特許文献４では、原料硫安の一部にワックスや界面活性剤などの固結防止剤を添加してから、残りの硫安を混合して圧縮造粒することで固結防止材の表面分布を不均一として固結を防止しているが、この方法では、固結防止材が必要であるうえに、固結防止材と硫安の混合工程に加えて混合物と硫安との混合工程がさらに必要となる。特許文献５では、粒状窒素肥料にトレハロースなど糖類を溶質とする溶液を混合することで粒状窒素肥料を被覆し、水分の吸収及び放出を抑制して固結防止しているが、固結防止材の添加のための工程や固結防止材のコストが必要となる。 As described above, various granular nitrogen fertilizers and methods for producing the same have been proposed. For caking that becomes a problem during long-term storage of granular nitrogen fertilizers, an anti-caking material is added as a preventive measure. However, sufficient effects are not obtained. In addition, the addition of the anti-caking material requires an additional step, which increases the cost. Patent Document 1 describes that a granular product has a large particle size and thus a high crushing strength and a low specific surface area, so that moisture is low and caking does not easily occur. However, the crushing strength is high and the specific surface area is low. If the water content is low, the water content is not necessarily low. If the water content is high, solidification occurs even if the particle size is large. In Patent Document 2, the crystal grain size is selected and granulated. However, the purpose is to isolate the intermediate size without granulation, and there is no effect in preventing caking. Further, Patent Document 2 describes the use of an additive that affects physical characteristics, but additional steps and additional costs are required even if an anti-caking material is added. In Patent Document 3, it is described that fine ammonium sulfate obtained by classification after granulation is mixed with raw material ammonium sulfate and granulated to make the ammonium sulfate difficult to disintegrate. In addition to the contents being implemented, there is no description on the effect of preventing caking, and caking occurs if the moisture is high as in Patent Document 1. In Patent Document 4, the surface distribution of the anti-caking material is reduced by adding an anti-caking agent such as a wax or a surfactant to a part of the raw ammonium sulfate, and then mixing the remaining ammonium sulfate and performing compression granulation. Although the caking is prevented as uniform, this method requires an anti-caking material and further requires a mixing step of the mixture and ammonium sulfate in addition to the mixing step of the anti-caking material and ammonium sulfate. . In Patent Document 5, granular nitrogenous fertilizer is coated with granular nitrogenous fertilizer by mixing a solution containing saccharides such as trehalose as a solute, and the absorption and release of moisture is suppressed to prevent caking. The cost for the process for the addition of anti-caking and the anti-caking material is required.
本発明は、前記課題を解決するために鋭意検討した結果、原料として、二次元Ｘ線回折したとき、入射Ｘ線の方向と検出器の方向のなす角２θ＝７２．３°における配向度が０．９９５以上となる細粒結晶硫安を６０ｗｔ％以上含む原料を使用することで、水分含有量が低くてアンモニア性窒素含有量が高く、保管時の固結性が低い粒状窒素肥料を得ることができることを見出した。 As a result of intensive studies to solve the above-mentioned problems, the present invention has a degree of orientation at an angle 2θ = 72.3 ° formed by the direction of the incident X-ray and the direction of the detector when two-dimensional X-ray diffraction is performed as a raw material. To obtain a granular nitrogen fertilizer having a low moisture content, a high ammoniacal nitrogen content, and a low caking property during storage by using a raw material containing 60 wt% or more of fine crystal ammonium sulfate of 0.995 or more I found out that I can.
上記目的を達成するために、本発明は以下の構成を採用する。すなわち、
１．二次元Ｘ線回折測定において入射Ｘ線の方向と検出器の方向のなす角２θ＝７２．３°における配向度が０．９９５以上である細粒結晶硫安を６０ｗｔ％以上含むことを特徴とする粒状窒素肥料。
２．細粒結晶硫安の粒径が１．７ｍｍ以下であり、水分含有率が０．３ｗｔ％以下であり、かつアンモニア性窒素含有率が２０．５％以上である、１に記載の粒状窒素肥料。
３．圧壊強度が３．０ｋｇｆ以上である、１または２に記載の粒状窒素肥料。
４．粒状窒素肥料７５０ｇを６０ｋｇの錘で１ヶ月荷重をかけた後の固結率が２０％以下である１〜３のいずれかに記載の粒状窒素肥料。
５．固結強度が０．５ｋｇ／ｃｍ２以下である、１〜４のいずれかに記載の粒状窒素肥料。
６．表面にタルク、ポリエチレングリコール、ステアリン酸金属塩、ラウリル硫酸金属塩、カオリン、炭酸カルシウム、酸化ケイ素、テレフタル酸カルシウム、酸化アルミニウム、酸化チタン、リン酸カルシウム、およびフッ化リチウムから選ばれる少なくとも一種の固結防止材を含む、１〜５のいずれかに記載の粒状窒素肥料。
７．１〜６のいずれかに記載の粒状窒素肥料と、リン成分を含有する粒状肥料および／またはカリウム成分を含有する粒状肥料とを含む混合肥料。
８．下記の工程１）〜３）を含む、６に記載の粒状窒素肥料の製造方法、
１）二次元Ｘ線回折測定において入射Ｘ線の方向と検出器の方向のなす角２θ＝７２．３°における配向度が０．９９５以上である細粒結晶硫安を６０ｗｔ％以上含む原料を造粒して粒状物を得る造粒工程、
２）１）で得られた粒状物を整粒して形状を調節する整粒工程、
３）２）で整粒された粒状物にタルク、ポリエチレングリコール、ステアリン酸金属塩、ラウリル硫酸金属塩、カオリン、炭酸カルシウム、酸化ケイ素、テレフタル酸カルシウム、酸化アルミニウム、酸化チタン、リン酸カルシウム、およびフッ化リチウムから選ばれる少なくとも一種の固結防止材を添加し被覆する被覆工程。
９．圧縮成型方式で原料を造粒する、８に記載の粒状窒素肥料の製造方法。
１０．一対のローラーを用いたブリケット方式により原料を圧縮して造粒する、８に記載の粒状窒素肥料の製造方法。
１１．カプロラクタム硫酸塩にアンモニアを添加してカプロラクタムと硫安水溶液を得た後、硫安水溶液を圧力１０．１ｋＰａ ａｂｓ以上で晶析して原料を造粒する、８に記載の粒状窒素肥料の製造方法。
１２．下記の工程１）〜３）を含む、１〜５のいずれかに記載の粒状窒素肥料の製造方法、
１）二次元Ｘ線回折測定において入射Ｘ線の方向と検出器の方向のなす角２θ＝７２．３°における配向度が０．９９５以上である細粒結晶硫安を６０ｗｔ％以上含む原料を造粒して粒状物を得る造粒工程、
２）１）で得られた粒状物を整粒し形状を調節する整粒工程、
３）２）で整粒された粒状物を乾燥する乾燥工程。
１３．圧縮成型方式で原料を造粒する、１２に記載の粒状窒素肥料の製造方法。
１４．一対のローラーを用いたブリケット方式により原料を圧縮して造粒する、１２に記載の粒状窒素肥料の製造方法。
１５．カプロラクタム硫酸塩にアンモニアを添加してカプロラクタムと硫安水溶液を得た後、硫安水溶液を圧力１０．１ｋＰａ ａｂｓ以上で晶析して原料を造粒する、１２に記載の粒状窒素肥料の製造方法。
In order to achieve the above object, the present invention adopts the following configuration. That is,
1. In the two-dimensional X-ray diffraction measurement, 60 wt% or more of fine crystal ammonium sulfate having an orientation degree of 0.995 or more at an angle 2θ = 72.3 ° formed by the direction of incident X-rays and the direction of the detector is included. Granular nitrogen fertilizer.
2. 2. The granular nitrogen fertilizer according to 1, wherein the particle size of the fine crystal ammonium sulfate is 1.7 mm or less, the water content is 0.3 wt% or less, and the ammoniacal nitrogen content is 20.5% or more.
3. The granular nitrogen fertilizer according to 1 or 2, having a crushing strength of 3.0 kgf or more.
4). The granular nitrogen fertilizer according to any one of 1 to 3, wherein a consolidation rate after applying 750 g of granular nitrogen fertilizer with a weight of 60 kg for one month is 20% or less.
5. The granular nitrogenous fertilizer in any one of 1-4 whose consolidation strength is 0.5 kg / cm < 2 > or less.
6). At least one caking prevention selected from talc, polyethylene glycol, metal stearate, metal lauryl sulfate, kaolin, calcium carbonate, silicon oxide, calcium terephthalate, aluminum oxide, titanium oxide, calcium phosphate and lithium fluoride on the surface The granular nitrogen fertilizer in any one of 1-5 containing a material.
The mixed fertilizer containing the granular nitrogenous fertilizer in any one of 7.1-6, the granular fertilizer containing a phosphorus component, and / or the granular fertilizer containing a potassium component.
8). The manufacturing method of the granular nitrogen fertilizer of 6 containing the following process 1) -3),
1) In a two-dimensional X-ray diffraction measurement, a raw material containing 60 wt% or more of fine crystal ammonium sulfate having an orientation degree of 0.995 or more at an angle 2θ = 72.3 ° between the direction of incident X-rays and the direction of the detector is prepared. Granulation process to obtain granules by granulation,
2) A sizing step of sizing the granular material obtained in 1) to adjust the shape,
3) Talc, polyethylene glycol, metal stearate, metal lauryl sulfate, kaolin, calcium carbonate, silicon oxide, calcium terephthalate, aluminum oxide, titanium oxide, calcium phosphate, and fluoride to the granulated particles in 2) A coating step of adding and coating at least one anti-caking material selected from lithium.
9. 9. The method for producing granular nitrogen fertilizer according to 8, wherein the raw material is granulated by a compression molding method.
10. The manufacturing method of the granular nitrogen fertilizer of 8 which compresses and granulates a raw material with the briquette system using a pair of roller.
11. 9. The method for producing granular nitrogen fertilizer according to 8, wherein ammonia is added to caprolactam sulfate to obtain caprolactam and an aqueous ammonium sulfate solution, and then the aqueous ammonium sulfate solution is crystallized at a pressure of 10.1 kPa abs or more to granulate the raw material.
12 The manufacturing method of the granular nitrogen fertilizer in any one of 1-5 containing the following process 1) -3),
1) In a two-dimensional X-ray diffraction measurement, a raw material containing 60 wt% or more of fine crystal ammonium sulfate having an orientation degree of 0.995 or more at an angle 2θ = 72.3 ° between the direction of incident X-rays and the direction of the detector is prepared. Granulation process to obtain granules by granulation,
2) A sizing step of sizing the granular material obtained in 1) to adjust the shape,
3) A drying step of drying the granulated particles in 2).
13. 13. The method for producing granular nitrogen fertilizer according to 12, wherein the raw material is granulated by a compression molding method.
14 13. The method for producing granular nitrogen fertilizer according to 12, wherein the raw material is compressed and granulated by a briquette method using a pair of rollers.
15. 13. The method for producing granular nitrogen fertilizer according to 12, wherein ammonia is added to caprolactam sulfate to obtain caprolactam and an aqueous ammonium sulfate solution, and then the aqueous ammonium sulfate solution is crystallized at a pressure of 10.1 kPa abs or more to granulate the raw material.
本発明によれば、低水分、高アンモニア性窒素の細粒結晶硫安を含む粒状窒素肥料とすることで、粒状窒素肥料の粒硬度が高く、かつ保管時に固結しにくい粒状窒素肥料を得ることができる。 According to the present invention, by using a granular nitrogen fertilizer containing fine crystal ammonium sulfate of low moisture and high ammoniacal nitrogen, it is possible to obtain a granular nitrogen fertilizer having high granular hardness of the granular nitrogen fertilizer and difficult to consolidate during storage. Can do.
＜細粒結晶硫安＞
細粒結晶硫安は、カプロラクタムの製造において、カプロラクタム硫酸塩にアンモニアを添加してカプロラクタムと硫酸アンモニウムを得た後に、カプロラクタム水溶液と硫安水溶液を分離して得られる硫安水溶液や、コークス炉ガスを硫酸と接触させて得られる硫安水溶液から、晶析により結晶化されたものであり、結晶と母液の分離については、公知の方式で行われる。例えば、遠心によって液体から分離した後、場合によっては、結晶を乾燥することで得られる。細粒結晶硫安は、晶析時に過飽和度が高すぎると結晶が急激に凝集して母液を取り込み、粒径が大きく、水分が高く、不純物が多くなるため、圧力１０．１ｋＰａ ａｂｓ以上の圧力として晶析することで、結晶配向した、結晶性の高い細粒結晶硫安を得ることができる。結晶性の高さは、二次元Ｘ線回折を行うことで測定することができ、測定結果から求められる配向度が０．９９５以上であることが好ましい。さらに好ましくは配向度が０．９９７以上であり、配向度が１．０であれば、結晶性が最も高い場合であり、最も好ましい。また細粒結晶硫安を含む割合は、６０ｗｔ％以上が好ましく、さらに好ましくは８０％以上であり、１００％であれば、結晶性の高い細粒結晶硫安のみとなり、最も好ましい。なお、配向度とは、結晶の揃い具合を示す指標であり、二次元Ｘ線回折において、あおり角χ（°）に応じて得られた配向性ピークの半値幅（°）より下記式（１）で示される。
<Fine crystal ammonium sulfate>
In the production of caprolactam, fine-grained ammonium sulfate is obtained by adding ammonia to caprolactam sulfate to obtain caprolactam and ammonium sulfate, and then contacting the aqueous solution of ammonium sulfate obtained by separating caprolactam aqueous solution and ammonium sulfate aqueous solution with coke oven gas with sulfuric acid. It is crystallized from the aqueous ammonium sulfate solution obtained by crystallization by crystallization, and the separation of the crystal and the mother liquor is carried out by a known method. For example, after separation from the liquid by centrifugation, in some cases, the crystals are dried. In the case of fine ammonium sulfate, if the supersaturation is too high during crystallization, the crystals agglomerate rapidly and the mother liquor is taken in. The particle size is large, the moisture is high, and the amount of impurities increases. Therefore, the pressure is 10.1 kPa abs or more. By crystallizing, it is possible to obtain crystallographically oriented fine crystal ammonium sulfate. The height of crystallinity can be measured by performing two-dimensional X-ray diffraction, and the degree of orientation obtained from the measurement result is preferably 0.995 or more. More preferably, the degree of orientation is 0.997 or more, and if the degree of orientation is 1.0, the crystallinity is the highest and the most preferable. Further, the ratio of containing fine crystal ammonium sulfate is preferably 60 wt% or more, more preferably 80% or more, and 100% is most preferable because only fine crystal ammonium sulfate having high crystallinity is obtained. The degree of orientation is an index indicating the degree of alignment of crystals. In two-dimensional X-ray diffraction, the following formula (1) is obtained from the half-value width (°) of the orientation peak obtained according to the tilt angle χ (°). ).
配向度＝（１８０−配向性ピーク半値幅）／１８０・・・（１） Degree of orientation = (180−full width at half maximum of orientation) / 180 (1)
また細粒結晶硫安の粒径は、結晶同士が凝集して母液を取り込んでいない小さい粒径ほど固結性の改善につながるため、１．７ｍｍ以下が好ましい。より好ましくは、１．４ｍｍ以下であり、さらに好ましくは１．１８ｍｍ以下である。細粒結晶硫安の粒径は、篩い（目開き１０メッシュ＝１．７ｍｍ、１２メッシュ＝１．４ｍｍ、１４メッシュ＝１．１８ｍｍ）で分級して求めることができる。 In addition, the particle size of the fine crystal ammonium sulfate is preferably 1.7 mm or less because the smaller the particle size in which the crystals are aggregated and the mother liquor is not taken in, the better the consolidation is. More preferably, it is 1.4 mm or less, More preferably, it is 1.18 mm or less. The particle size of the fine crystal ammonium sulfate can be determined by classification with a sieve (aperture 10 mesh = 1.7 mm, 12 mesh = 1.4 mm, 14 mesh = 1.18 mm).
＜粒状窒素肥料＞
本発明では、粒状窒素肥料は、配向度の高い細粒結晶硫安を原料として使用することにより、低水分で、高アンモニア性窒素含有量とし、固結性を改善することができる。
<Granular nitrogen fertilizer>
In the present invention, the granular nitrogen fertilizer can have a high ammoniacal nitrogen content with a low moisture content by using fine crystal ammonium sulfate having a high degree of orientation as a raw material, and can improve the caking property.
粒状窒素肥料の水分率は、長期保管中の粒状肥料組成物同士の固結を防止する観点で０．３％以下であることが好ましい。より好ましくは０．２％以下であり、さらに好ましくは０．１％以下であり、完全に水分を乾燥させた０％であれば全く固結しないため最も好ましい。なお、粒状肥料組成物の水分率は、公定肥料分析法に従い加熱減量法で測定した値である。 The moisture content of the granular nitrogen fertilizer is preferably 0.3% or less from the viewpoint of preventing caking between the granular fertilizer compositions during long-term storage. More preferably, it is 0.2% or less, and further preferably 0.1% or less. If it is 0% with completely dried water, it is most preferable because it does not solidify at all. In addition, the moisture content of a granular fertilizer composition is the value measured by the heat loss method according to the official fertilizer analysis method.
粒状窒素肥料のアンモニア性窒素は、単位重量当たりの窒素源としての肥料効果の面から、２０．５％以上が好ましく、２１．０％以上がさらに好ましい。 Ammonia nitrogen in the granular nitrogen fertilizer is preferably 20.5% or more, and more preferably 21.0% or more from the viewpoint of fertilizer effect as a nitrogen source per unit weight.
粒状窒素肥料の粒径は、機械施肥において、肥料の到達距離を確保するため、２〜４ｍｍが好ましい。より好ましくは２．５〜３．５ｍｍである。 The particle size of the granular nitrogen fertilizer is preferably 2 to 4 mm in order to ensure the reach of the fertilizer in mechanical fertilization. More preferably, it is 2.5 to 3.5 mm.
粒状窒素肥料の形状は、機械施肥をした場合、作物の葉などに付着せず土壌に落下するよう丸形状であることが好ましい。丸形状ではない、例えば平らな形状の圧片肥料であると、葉に付着して落下せず栄養分供給が乏しくなる恐れがある。粒状肥料組成物の粒径は、篩い分けを行って測定する。 The shape of the granular nitrogen fertilizer is preferably a round shape so that it falls on the soil without attaching to the leaves of the crop when mechanical fertilization is applied. If it is not a round shape, for example, it is a flat-shaped pressed piece fertilizer, it will adhere to the leaf and will not fall, and the supply of nutrients may be poor. The particle size of the granular fertilizer composition is measured by sieving.
粒状窒素肥料の粒硬度（圧壊強度）は、３〜５ｋｇｆの範囲であることが好ましい。粒硬度（圧壊強度）が３ｋｇｆ未満であると、製造時に粒状窒素肥料が粉化しやすく、製造時の収率が低下する。また、粒状窒素肥料の保管中にも粉化が発生しやすく、粒状物同士の固結の原因となる。一方、粒硬度（圧壊強度）が５ｋｇｆを越える場合は、土壌中での粒状窒素肥料の崩壊性が悪く、肥効が低下する。より好ましくは３〜４．５ｋｇｆの範囲であり、さらに好ましくは３．５〜４．５ｋｇｆの範囲である。なお、粒状窒素肥料の粒硬度（圧壊強度）の測定にあたっては、木屋式硬度計で２０粒を測定し、その測定結果の平均値を粒硬度（圧壊強度）とする。 The granular hardness (crushing strength) of the granular nitrogen fertilizer is preferably in the range of 3 to 5 kgf. When the grain hardness (crushing strength) is less than 3 kgf, the granular nitrogen fertilizer tends to be pulverized during production, and the yield during production decreases. In addition, pulverization is likely to occur during storage of the granular nitrogen fertilizer, which causes caking of the granular materials. On the other hand, when the grain hardness (crushing strength) exceeds 5 kgf, the disintegration property of the granular nitrogen fertilizer in the soil is poor and the fertilization effect is reduced. More preferably, it is the range of 3-4.5 kgf, More preferably, it is the range of 3.5-4.5 kgf. In measuring the grain hardness (crushing strength) of granular nitrogen fertilizer, 20 grains are measured with a Kiyama-type hardness meter, and the average value of the measurement results is taken as the grain hardness (crushing strength).
粒状窒素肥料の収率は、造粒時および整粒時の肥料組成物の廃棄量をできるだけ削減するため、あるいは廃棄せずに造粒工程へリサイクルするためには５５％以上であることが好ましい。より好ましくは７０％以上であり、さらに好ましくは８０％以上であり、完全に回収できた場合１００％が最も好ましい。なお、収率とは、投入原料の重量に対する造粒および整粒して得られた粒状窒素肥料の重量であって、下記式（２）で示される。 The yield of granular nitrogen fertilizer is preferably 55% or more in order to reduce the amount of fertilizer composition discarded during granulation and sizing as much as possible or to recycle to the granulation process without discarding. . More preferably, it is 70% or more, further preferably 80% or more, and 100% is most preferable when it can be completely recovered. The yield is the weight of the granular nitrogen fertilizer obtained by granulation and sizing with respect to the weight of the input raw material, and is represented by the following formula (2).
収率＝（粒状窒素肥料の重量）／（投入原料重量）×１００（％）・・・（２） Yield = (weight of granular nitrogen fertilizer) / (input raw material weight) × 100 (%) (2)
粒状窒素肥料の固結強度は、０．５ｋｇ／ｃｍ２以下であることが好ましい。０．５ｋｇ／ｃｍ２以上であると、例えば固結部分がフレキシブルコンテナバッグから流れ出ないため、ホッパーに投入することが容易ではない、あるいは機械施肥において生育させる植物まで粒状窒素肥料をまくことができないなど、取り扱い性に劣る恐れがある。より好ましくは固結強度が０．３ｋｇ／ｃｍ２以下であり、さらに好ましくは０．１ｋｇ／ｃｍ２以下である。なお、固結強度は、山中式土壌硬度計を使用して針部を肥料上面に対して垂直に圧入して測定した値である。 The consolidation strength of the granular nitrogen fertilizer is preferably 0.5 kg / cm 2 or less. If it is 0.5 kg / cm 2 or more, for example, the consolidated portion does not flow out of the flexible container bag, so it is not easy to put into the hopper, or the granular nitrogen fertilizer cannot be planted up to plants grown in mechanical fertilization There is a risk of poor handling. More preferably consolidation strength is 0.3 kg / cm 2 or less, more preferably 0.1 kg / cm 2 or less. The consolidation strength is a value measured by pressing the needle portion perpendicularly to the upper surface of the fertilizer using a Yamanaka type soil hardness meter.
粒状窒素肥料の取り扱いを容易にするため固結率は２０％以下であることが好ましい。固結率が２０％を越えると上記と同様に流動性が悪くなったり、機械施肥ができない恐れがある。より好ましくは１５％以下であり、さらに好ましくは１０％以下であり、全く固結がない０％が最も好ましい。なお、固結率は粒状窒素肥料７５０ｇに対して６０ｋｇの錘で一ヶ月荷重後の粒状肥料組成物のうち固結部分重量の割合であり、下記式（３）で示される。 In order to facilitate the handling of the granular nitrogen fertilizer, the consolidation rate is preferably 20% or less. If the consolidation rate exceeds 20%, the fluidity may deteriorate as described above, or mechanical fertilization may not be possible. More preferably, it is 15% or less, more preferably 10% or less, and most preferably 0% which does not cause any solidification. In addition, a consolidation rate is a ratio of a solidification part weight among the granular fertilizer compositions after a one-month load with a weight of 60 kg with respect to 750 g of granular nitrogen fertilizer, and is shown by following formula (3).
固結率＝（一ヶ月間荷重後の固結部分重量（ｇ））／７５０×１００ ・・・（３） Consolidation rate = (Consolidated part weight (g) after one month load) / 750 × 100 (3)
本発明で得られた粒状窒素肥料は、固結防止材としてタルク、ポリエチレングリコール、ステアリン酸金属塩、ラウリル硫酸金属塩、カオリン、炭酸カルシウム、酸化ケイ素、テレフタル酸カルシウム、酸化アルミニウム、酸化チタン、リン酸カルシウム、およびフッ化リチウムから選ばれる少なくとも一種を表面に含むことができる。また、リン成分を含有する粒状肥料組成物および／またはカリウム成分を含有する粒状肥料組成物をドライブレンドして得られる混合肥料として使用ができる。この混合肥料は任意の割合でブレンドできるため、作物毎に対応したブレンドを行うことができる。 The granular nitrogen fertilizer obtained in the present invention contains talc, polyethylene glycol, metal stearate, metal lauryl sulfate, kaolin, calcium carbonate, silicon oxide, calcium terephthalate, aluminum oxide, titanium oxide and calcium phosphate as anti-caking materials. , And at least one selected from lithium fluoride can be included on the surface. Moreover, it can be used as a mixed fertilizer obtained by dry blending a granular fertilizer composition containing a phosphorus component and / or a granular fertilizer composition containing a potassium component. Since this mixed fertilizer can be blended at an arbitrary ratio, blending corresponding to each crop can be performed.
＜粒状窒素肥料の製造方法＞
粒状窒素肥料の造粒方法は、圧縮造粒が好ましく、圧縮造粒装置は、タブレット方式、板状方式、ブリケット方式の何れを用いても問題ないが、タブレット方式では生産効率が低く粒状窒素肥料の大量生産が困難であり、また板状方式では球形でバリの少ない造粒窒素肥料を生産することが困難であるため、ブリケット方式を用いることが好ましい。ブリケット方式の圧縮造粒装置としては、例えばブリケッタ（登録商標）ＢＳＳ型（新東工業製）などを好ましく用いることができる。
<Production method of granular nitrogen fertilizer>
The granulation method for granular nitrogen fertilizer is preferably compression granulation, and the compression granulation apparatus may be any of the tablet method, plate method, and briquette method, but the tablet method has low production efficiency and granular nitrogen fertilizer. It is preferable to use the briquette method because it is difficult to produce a large amount of the product, and it is difficult to produce a granulated nitrogen fertilizer having a spherical shape and few burrs by the plate method. As a briquette type compression granulator, for example, a Briquetta (registered trademark) BSS type (manufactured by Shinto Kogyo) or the like can be preferably used.
原料の細粒結晶硫安を圧縮造粒装置に供給する方法は、特に制限はされないが、例えば細粒結晶硫安をホッパーに貯蔵し、ホッパーに付帯した搬送コンベアより造粒装置に直接供給、またはホッパー搬送コンベアからベルトコンベアやバケットコンベア等を経由して造粒装置へ供給することができる。 The method for supplying the raw material fine crystal ammonium sulfate to the compression granulator is not particularly limited. For example, the fine crystal ammonium sulfate is stored in a hopper and directly supplied to the granulator from a conveyor conveyer attached to the hopper, or the hopper It can be supplied from the conveyor to the granulator via a belt conveyor or a bucket conveyor.
造粒圧力とは、原料の細粒結晶硫安に加わる総荷重を有効幅で除算した値（線圧）を示し、有効幅とは、原料の細粒結晶硫安に荷重が加わる部分における、圧縮機側の長径を示す。例えば、タブレット方式であれば有効幅はタブレット部分の長径であり、ローラーを用いたブリケット方式であれば、有効幅はローラーにて原料の細粒結晶硫安が圧縮されている部分の長さである。造粒圧力は、０．６〜３０．０ｋＮ／ｃｍの範囲内にあることが好ましく、より好ましくは３．０〜２０．０ｋＮ／ｃｍであり、さらに好ましくは、５．０〜１５．０ｋＮ／ｃｍである。造粒圧力が上記を超えて低くなると、圧力不足のため、細粒結晶硫安の造粒自体が起こらない恐れがある。造粒圧力が上記を超えて高くなると、圧縮造粒機に必要以上の荷重がかかるため、装置寿命が著しく低下する恐れがある。 The granulation pressure indicates the value (linear pressure) obtained by dividing the total load applied to the raw material fine crystal ammonium sulfate by the effective width, and the effective width is the compressor in the portion where the load is applied to the raw material fine crystal ammonium sulfate. The major axis on the side is shown. For example, if the tablet method, the effective width is the long diameter of the tablet part, if the briquette method using a roller, the effective width is the length of the portion where the fine crystal ammonium sulfate of the raw material is compressed by the roller . The granulation pressure is preferably in the range of 0.6 to 30.0 kN / cm, more preferably 3.0 to 20.0 kN / cm, and still more preferably 5.0 to 15.0 kN / cm. cm. If the granulation pressure is lower than the above, there is a possibility that granulation of fine crystal ammonium sulfate does not occur due to insufficient pressure. If the granulation pressure is higher than the above, an excessive load is applied to the compression granulator, which may significantly reduce the device life.
圧縮造粒機のバリ厚みとは、原料の細粒結晶硫安に荷重が加わる部分における原料の細粒結晶硫安の短径を示す。例えばタブレット方式であれば、バリ厚みはタブレット部分の短径であり、ローラーを用いたブリケット方式であれば、バリ厚みはロール間距離（クリアランス）の最も短い長さのことである。バリ厚みは、１．００〜２．５０ｍｍの範囲内にあることが好ましく、１．２０〜２．００ｍｍの範囲内にあることがより好ましい。バリ厚みが上記を超えて低くなると、粒状窒素肥料の圧壊強度・収量ともに低下する傾向にある。バリ厚みが上記を超えて高くなると、粒状窒素肥料の形状が肥料散布に不適となることや、造粒した粒状窒素肥料を、例えば解砕ボールを用いた振動篩で解砕し粒径を揃える場合、篩いの目詰まりの原因となる恐れがある。 The burr thickness of the compression granulator indicates the short diameter of the raw material fine crystal ammonium sulfate in a portion where a load is applied to the raw material fine crystal ammonium sulfate. For example, in the case of a tablet system, the burr thickness is the short diameter of the tablet part, and in the case of a briquette system using a roller, the burr thickness is the length of the shortest distance between the rolls (clearance). The burr thickness is preferably in the range of 1.00 to 2.50 mm, and more preferably in the range of 1.20 to 2.00 mm. When the burr thickness is lower than the above, both the crushing strength and yield of the granular nitrogen fertilizer tend to decrease. If the burr thickness exceeds the above, the shape of the granular nitrogen fertilizer becomes unsuitable for fertilizer application, and the granulated granular nitrogen fertilizer is crushed with, for example, a vibrating sieve using a pulverizing ball to make the particle size uniform In this case, it may cause clogging of the sieve.
単位時間・単位長さあたりの造粒機が処理可能な原料の細粒結晶硫安（以下造粒効率と称する）とは、造粒機に供給した原料の細粒結晶硫安を１時間あたりの供給量に換算し、さらに有効幅にて除算した、単位時間・単位長さあたりの造粒能力を示す。 The raw granular ammonium sulfate that can be processed by the granulator per unit time and unit length (hereinafter referred to as granulation efficiency) is the supply of fine granular ammonium sulfate supplied to the granulator per hour. It shows the granulation capacity per unit time and unit length, which is converted into a quantity and further divided by the effective width.
圧縮造粒機で造粒した粒状窒素肥料は、解砕、整粒、分級を行うことで、肥料として好ましい形状の粒状窒素肥料を得ることができる。 The granular nitrogen fertilizer granulated by the compression granulator can obtain a granular nitrogen fertilizer having a preferable shape as a fertilizer by performing crushing, granulating and classifying.
粒径の揃った粒状窒素肥料を得るために、解砕機を用いて圧縮造粒後の粒状窒素肥料を解砕することが好ましい。解砕機の種類に特に制限は無く、例えば、ジョークラッシャー・ロールクラッシャーなどの各種クラッシャーや、ローラーミル・カッティングミルなどの各種ミル、解砕メディアを添加した振動篩などが好ましく用いられる。また、これらの解砕機を組み合わせて用いることも可能である。 In order to obtain a granular nitrogen fertilizer having a uniform particle size, it is preferable to crush the granular nitrogen fertilizer after compression granulation using a crusher. There are no particular limitations on the type of crusher, and various crushers such as a jaw crusher and a roll crusher, various mills such as a roller mill and a cutting mill, and a vibration sieve to which crushing media are added are preferably used. It is also possible to use these crushers in combination.
球形でバリの少ない粒状窒素肥料を得るために、整粒機を用いて整粒することが好ましい。整粒機の種類に特に制限はなく、例えば高速転動方法、オシレータ式、架砕方式、遠心回転方式などが好ましく用いられ、高速転動方式の球形整粒機であるマルメライザー（登録商標：ダルトン製）を用いて粒状窒素肥料を整粒することがより好ましい。 In order to obtain a spherical nitrogen fertilizer with few burrs, it is preferable to use a particle sizer. There is no particular limitation on the type of the granulator, for example, a high-speed rolling method, an oscillator type, a crushing method, a centrifugal rotating method, or the like is preferably used, and Malmerizer (registered trademark: a high-speed rolling type spherical granulator). More preferably, the granular nitrogen fertilizer is sized using a Dalton product.
整粒機の処理時間は、０．２〜５．０分の範囲内にあることが好ましく、０．３〜３．０分の範囲内であることがより好ましい。整粒機の処理時間が上記を超えて低くなると、粒状窒素肥料のバリ除去が不十分となる恐れがある。整粒機の処理時間が上記を超えて高くなると、バリ以外の部分が切削される量が増加し、粒状窒素肥料の収量が低下する恐れがある。さらに整粒処理に必要な時間が多くなるため、単位時間あたりの造粒状窒素肥料収量も低下する恐れがある。 The processing time of the granulator is preferably in the range of 0.2 to 5.0 minutes, and more preferably in the range of 0.3 to 3.0 minutes. If the processing time of the granulator becomes lower than the above, there is a risk that the burr removal of the granular nitrogen fertilizer will be insufficient. If the processing time of the granulator becomes higher than the above, the amount of parts other than burrs that are cut increases, and the yield of granular nitrogen fertilizer may decrease. Furthermore, since the time required for the sizing treatment is increased, the yield of granulated nitrogen fertilizer per unit time may be reduced.
整粒機の回転速度は、５０〜２０００回転／分の範囲内にあることが好ましく、１００〜１５００回転／分の範囲内にあることがより好ましい。整粒機の回転速度が上記の範囲より低くなると、粒状窒素肥料のバリ除去が不十分となり、さらに整粒処理に必要な時間が多くなるため、単位時間あたりの粒状窒素肥料収量も低下する恐れがある。整粒機の回転速度が上記の範囲を超えて高くなると、騒音増加および機器寿命の低下といった問題が生ずる恐れがある。 The rotational speed of the granulator is preferably in the range of 50 to 2000 revolutions / minute, and more preferably in the range of 100 to 1500 revolutions / minute. If the rotational speed of the granulator becomes lower than the above range, the removal of burrs on the granular nitrogen fertilizer will be insufficient, and the time required for the sizing process will increase, which may reduce the yield of granular nitrogen fertilizer per unit time. There is. If the rotational speed of the granulator becomes higher than the above range, problems such as an increase in noise and a decrease in equipment life may occur.
所定の粒径以上の粒状窒素肥料を得るために、分級機を用いて粒状窒素肥料を分級することが望ましい。乾式分級が可能なものであれば、分級機の種類に特に制限はないが、振動篩を用いることが好ましい。篩の目開きは、所定の粒径を得られる大きさであれば特に制限はないが、１．８〜２．２ｍｍ、および３．８〜４．２ｍｍの目開きであることが好ましく、これら目開きを有する篩を組み合わせて粒径２．０〜４．０ｍｍの粒状窒素肥料を得る分級方法が好ましい。 In order to obtain a granular nitrogen fertilizer having a predetermined particle size or more, it is desirable to classify the granular nitrogen fertilizer using a classifier. The type of classifier is not particularly limited as long as dry classification is possible, but it is preferable to use a vibration sieve. The opening of the sieve is not particularly limited as long as a predetermined particle size can be obtained, but preferably 1.8 to 2.2 mm and 3.8 to 4.2 mm. A classification method for obtaining granular nitrogen fertilizer having a particle size of 2.0 to 4.0 mm by combining sieves having openings is preferable.
バリが少なく、圧壊強度が高く、窒素濃度が高く、粉塵の発生も少なく、固結が起こりづらい粒状窒素肥料を得るために、圧縮造粒機を用いて細粒結晶硫安を原料として造粒し、解砕機を用いて圧縮造粒後の粒状窒素肥料を解砕した後、球形整粒機を用いて解砕後の粒状窒素肥料を整粒し、分級機を用いて整粒の粒状窒素肥料を分級することが好ましい。各工程における粒状窒素肥料の輸送方法に制限はないが、自然落下・コンベア輸送・風送などを用いることが可能であり、コンベア輸送で原料である細粒結晶硫安を造粒機に輸送した後、自然落下で解砕機・球形整粒機・分級機へ輸送する方法が好ましい。これら輸送機器を含めた機器の接粉部分については、粒状窒素肥料に耐食性を持つ材質を用いることが好ましく、ＳＵＳ３１６Ｌまたは樹脂を用いることが好ましい。 In order to obtain granular nitrogen fertilizer that has few burrs, high crushing strength, high nitrogen concentration, low dust generation, and hardly caking, granulate fine ammonium sulfate using a compression granulator as a raw material. After pulverizing the granular nitrogen fertilizer after compression granulation using a crusher, the granular nitrogen fertilizer after pulverization using a spherical granulator is sized, and the granulated nitrogen nitrogen fertilizer using a classifier Is preferably classified. There are no restrictions on the method of transporting granular nitrogen fertilizer in each process, but it is possible to use natural fall, conveyor transport, air transport, etc., and after transporting the fine crystal ammonium sulfate that is the raw material to the granulator by conveyor transport A method of transporting to a crusher, spherical granulator, and classifier by natural fall is preferable. For the contact parts of equipment including these transportation equipment, it is preferable to use a material having corrosion resistance for granular nitrogen fertilizer, and it is preferable to use SUS316L or resin.
圧縮造粒機を用いて原料である細粒結晶硫安を造粒し、解砕機を用いて圧縮造粒後の粒状窒素肥料を解砕した際、また球形整粒機を用いて解砕後の粒状窒素肥料を整粒し、分級機を用いて整粒の粒状窒素肥料を分級した際に得られる篩下の微粉は、再度、原料である細粒結晶硫安中にリサイクルして混合し、造粒の原料として使用することができる。 When the granulated granular ammonium fertilizer is pulverized by using a compression granulator, the granular ammonium sulfate as a raw material is granulated, and the granulated nitrogen fertilizer is pulverized by using a pulverizer. The granular nitrogen fertilizer is sized, and the fine powder under the sieve obtained when the sized granular nitrogen fertilizer is classified using a classifier is recycled and mixed again into the raw material, fine crystal ammonium sulfate. It can be used as a raw material for grains.
造粒および整粒して粒状物を製造した後、粒状窒素肥料に、固結防止材としてタルク、ポリエチレングリコール、ステアリン酸金属塩、ラウリル硫酸金属塩、カオリン、炭酸カルシウム、酸化ケイ素、テレフタル酸カルシウム、酸化アルミニウム、酸化チタン、リン酸カルシウム、フッ化リチウムから選ばれる少なくとも一種を粒状窒素肥料表面に被覆して粒状窒素肥料とすることができる。被覆する方法としては、粒状窒素肥料を造粒および整粒し、分級機で分級した後に均一に被覆されていれば、分級機出口で添加してもよいし、ミキサーを用いて混合し被覆してもよいし、ベルトコンベア上で吹き付けを行って被覆してもよい。 After granulation and sizing to produce granules, pulverized nitrogen fertilizer, talc, polyethylene glycol, metal stearate, metal lauryl sulfate, kaolin, calcium carbonate, silicon oxide, calcium terephthalate as anti-caking agent The granular nitrogen fertilizer surface can be coated with at least one selected from aluminum oxide, titanium oxide, calcium phosphate, and lithium fluoride to form a granular nitrogen fertilizer. As a method of coating, granulated and fertilized granular nitrogen fertilizer, if it is uniformly coated after classification with a classifier, it may be added at the outlet of the classifier, or mixed and coated using a mixer. Alternatively, it may be coated by spraying on a belt conveyor.
粒状窒素肥料に対する固結防止材の添加量は、粒状窒素肥料１００重量部に対して０．０５〜０．５重量部が好ましく、装置への付着によるロスや、単位重量当たりの窒素含有量への影響がなく、肥料として崩壊性がよい硬度の肥料を得るためには粒状窒素肥料１００重量部に対して０．１〜０．３重量部がより好ましい。装置への付着ロスをより少なくするためには、粒状窒素肥料１００重量部に対して０．１５〜０．２５重量部がさらに好ましい。 The amount of the anti-caking material added to the granular nitrogen fertilizer is preferably 0.05 to 0.5 parts by weight with respect to 100 parts by weight of the granular nitrogen fertilizer, to the loss due to adhesion to the apparatus and the nitrogen content per unit weight In order to obtain a fertilizer with good hardness and good disintegration as a fertilizer, 0.1 to 0.3 parts by weight is more preferable with respect to 100 parts by weight of the granular nitrogen fertilizer. In order to reduce the adhesion loss to the apparatus, 0.15 to 0.25 parts by weight is more preferable with respect to 100 parts by weight of the granular nitrogen fertilizer.
造粒および整粒して粒状物を製造した後、粒状窒素肥料を乾燥して低水分化することも可能である。乾燥機の種類について特に制限はなく、回転式乾燥機、流動層乾燥機など熱風受熱式乾燥機や、攪拌乾燥機、赤外線加熱乾燥機など伝道伝熱型乾燥機が用いられるが、乾燥機の導入コストが低いことや、乾燥時の回転による整粒効果が見られることから、回転式乾燥機が好ましく用いられる。乾燥温度は、６０〜１５０℃が好ましく、さらに好ましくは、１００〜１３０℃である。乾燥温度が上記を超えて低くなると、乾燥による水分低減が不十分となり乾燥時間を長時間要して装置内部での粉化や生産性の悪化を招き、乾燥温度が上記を超えて高くなると、粒状窒素肥料の分解により、アンモニア性窒素濃度の低下を引き起こす恐れがある。乾燥時間は、５〜６０分が好ましく、さらに好ましくは、１０〜３０分である。乾燥時間が上記を超えて低くなると、乾燥効果が低く、水分低減が不十分となり、乾燥時間が上記を超えて高くなると、長時間加熱により装置内部での粉化や生産性の悪化を招く恐れがある。 After granulating and sizing to produce a granular material, it is possible to dry the granular nitrogen fertilizer to reduce moisture. There are no particular restrictions on the type of dryer, and hot-air heat-receiving dryers such as rotary dryers and fluidized bed dryers, and heat transfer type dryers such as stirring dryers and infrared heating dryers are used. A rotary drier is preferably used because the introduction cost is low and a sizing effect by rotation during drying is observed. The drying temperature is preferably 60 to 150 ° C, and more preferably 100 to 130 ° C. When the drying temperature is lower than the above, moisture reduction due to drying is insufficient, and it takes a long time to dry, resulting in pulverization and productivity deterioration inside the apparatus, and when the drying temperature is higher than the above, Degradation of granular nitrogen fertilizer may cause a decrease in ammoniacal nitrogen concentration. The drying time is preferably 5 to 60 minutes, and more preferably 10 to 30 minutes. If the drying time is lower than the above, the drying effect is low, moisture reduction is insufficient, and if the drying time is higher than the above, it may cause powdering inside the device or deterioration of productivity due to prolonged heating. There is.
本発明の実施例を以下に示すが、本発明は以下の実施例のみに限定されるものではない。ここで、実施例中の部数は重量部を示す。物性等の測定方法は以下のとおりである。 Examples of the present invention are shown below, but the present invention is not limited to the following examples. Here, the number of parts in the examples represents parts by weight. Measuring methods for physical properties and the like are as follows.
（１）粒径
粒径は、目開き２ｍｍおよび４ｍｍの篩いを使用して、下記式により２〜４ｍｍの粒径の割合を算出した。
２〜４ｍｍ粒径（％）＝粒径２〜４ｍｍの重量／篩い分けサンプル重量×１００
(1) Particle size The particle size was calculated using the following formula using a sieve with 2 mm openings and 4 mm sieves, and the ratio of the particle size of 2 to 4 mm was calculated.
2-4 mm particle size (%) = weight of particle size 2-4 mm / sieving sample weight × 100
（２）収率
投入原料（細粒結晶硫安＋篩い下微粉）の重量に対する造粒および整粒して得られた粒状窒素肥料の重量であって、下記式により算出した。
(2) Yield The weight of the granular nitrogen fertilizer obtained by granulation and sizing with respect to the weight of the input raw material (fine crystal ammonium sulfate + fine powder under sieve), and was calculated by the following formula.
収率（％）＝（粒状窒素肥料の重量）／（投入原料重量）×１００ Yield (%) = (weight of granular nitrogen fertilizer) / (input raw material weight) × 100
（２）粒硬度（圧壊強度）
木屋式硬度計で粒状窒素肥料２０粒それぞれの粒硬度（圧壊強度）を測定し、その平均を求めた値である。
(2) Grain hardness (crushing strength)
This is a value obtained by measuring the grain hardness (crushing strength) of each of the 20 granular nitrogen fertilizers using a Kiyama hardness tester, and calculating the average.
（３）アンモニア性窒素
公定肥料分析方法に定められたアンモニア性窒素測定方法のうち、アンモニウムイオンをヘキサチナレンテトラミンとし、遊離する酸を滴定するホルムアルデヒド法で測定した値である。
(3) Ammonia nitrogen It is the value measured by the formaldehyde method in which ammonium ion is hexatinalene tetramine and the free acid is titrated among the ammonia nitrogen measurement methods defined in the official fertilizer analysis method.
（４）水分率
粒状窒素肥料の水分率は、乾燥前の粒状窒素肥料を１３０℃で３時間乾燥後重量測定を行った際の加熱減量により求めた値であり、下記式で算出した。
(4) Moisture content The moisture content of the granular nitrogen fertilizer is a value obtained by weight loss after drying the granular nitrogen fertilizer before drying at 130 ° C. for 3 hours, and was calculated by the following formula.
水分率（％）＝（乾燥前の粒状窒素肥料重量−乾燥後の粒状窒素肥料重量）／（加熱前の粒状窒素肥料重量）×１００ Moisture content (%) = (weight of granular nitrogen fertilizer before drying−weight of granular nitrogen fertilizer after drying) / (weight of granular nitrogen fertilizer before heating) × 100
（５）固結強度
山中式土壌硬度計を使用して針部を肥料上面に対して垂直に圧入して測定した値である。
(5) Consolidation strength This is a value measured by pressing the needle part perpendicularly to the upper surface of the fertilizer using a Yamanaka soil hardness tester.
（６）固結率
粒状窒素肥料７５０ｇに対して６０ｋｇの錘で一ヶ月間荷重後の粒状窒素肥料のうち固結部分重量の割合であり、下記式で算出した。
(6) Consolidation rate It is the ratio of the solidified part weight of the granular nitrogenous fertilizer after one month load with a weight of 60 kg with respect to 750 g of granular nitrogenous fertilizer, and was calculated by the following formula.
固結率（％）＝（一ヶ月間荷重後の固結部分重量（ｇ））／７５０×１００ Consolidation rate (%) = (Consolidated part weight (g) after one month load) / 750 × 100
（実施例１）
配向度０．９９７の細粒結晶硫安１００重量部を原料とした。該原料を造粒機としてブリケッタ（登録商標）ＢＳＳ−ＩＨ型（新東工業製）に供給し、ロール有効幅を１５０ｍｍ、ロール圧力を８．３ｋＮ／ｃｍ、バリ厚みを１．７０ｍｍ、ポケットサイズを３．３ｍｍ、ローラー回転数８５ｒｐｍで造粒を行い、粗砕機にて破砕した後、目開き６．７ｍｍ、５．２ｍｍ、２．２ｍｍの篩いを有する３段解砕篩機（興和工業所製）に投入し、解砕メディア（ナイロン硬球ボール上段２００個、下段２００個）で解砕し、篩上品を回収した。続いて、マルメライザー（ダルトン製）に篩上解砕品を投入し、回転速度２２５ｒｐｍで１５秒間整粒処理を行った後に、目開き２ｍｍの篩を有する円形振動篩機（ダルトン製）に送り、分級を行った後、目開き２ｍｍの篩上品を粒状肥料組成物として回収した。粒状肥料組成物の２〜４ｍｍ粒径が９８．５％で、収率は５９．２％で、粒硬度（圧壊強度）は３．３ｋｇｆであった。また、粒状肥料組成物のアンモニア性窒素は２１．１％、水分率は０．２％、固結テスト１ヶ月後の固結率は９．０％、固結強度は０．２ｋｇ／ｃｍ２であった。
Example 1
The raw material was 100 parts by weight of fine-grained ammonium sulfate having an orientation degree of 0.997. The raw material is supplied to a Briquetta (registered trademark) BSS-IH type (manufactured by Shinto Kogyo) as a granulator, the effective roll width is 150 mm, the roll pressure is 8.3 kN / cm, the burr thickness is 1.70 mm, the pocket size Is granulated at 3.3 mm and with a roller rotation speed of 85 rpm, and crushed with a crusher, and then a three-stage crushing sieve machine having a sieve with openings of 6.7 mm, 5.2 mm, and 2.2 mm (Kowa Kogyo) Made into a product) and crushed with a crushing medium (200 nylon hard ball balls, 200 lower balls), and the sieved product was collected. Subsequently, the sieved crushed product is put into a Malmerizer (Dalton), subjected to a sizing process at a rotational speed of 225 rpm for 15 seconds, and then sent to a circular vibrating sieve (Dalton) having a sieve with a mesh opening of 2 mm. Then, the sieved product having an opening of 2 mm was collected as a granular fertilizer composition. The granular fertilizer composition had a 2-4 mm particle size of 98.5%, a yield of 59.2%, and a particle hardness (crushing strength) of 3.3 kgf. Moreover, the ammoniacal nitrogen of the granular fertilizer composition is 21.1%, the moisture content is 0.2%, the consolidation rate after one month of the consolidation test is 9.0%, and the consolidation strength is 0.2 kg / cm 2. Met.
（実施例２）
実施例１と同様の方法で粒状肥料組成物を作製した後、円形振動篩い工程において粒状窒素肥料１００重量部に対して０．２重量部のタルク（浅田製粉ＳＷ−Ａ）を添加して、粒状窒素肥料表面をタルクで被覆処理した。粒状窒素肥料組成物の２〜４ｍｍ粒径が９８．２％で、収率は５８．５％で、粒強度は３．２ｋｇｆであった。また、粒状窒素肥料組成物のアンモニア性窒素は２１．１％、水分率は０．２％、固結テスト１ヶ月後の固結率は４．０％、固結強度は０．１ｋｇ／ｃｍ２であった。
(Example 2)
After producing a granular fertilizer composition by the same method as in Example 1, 0.2 parts by weight of talc (Asada Flour Milling SW-A) is added to 100 parts by weight of granular nitrogen fertilizer in a circular vibration sieving step, The surface of granular nitrogen fertilizer was coated with talc. The 2-4 mm particle size of the granular nitrogen fertilizer composition was 98.2%, the yield was 58.5%, and the particle strength was 3.2 kgf. The granular nitrogen fertilizer composition has an ammoniacal nitrogen content of 21.1%, a moisture content of 0.2%, a consolidation rate after one month of consolidation test of 4.0%, and a consolidation strength of 0.1 kg / cm. 2 .
（実施例３）
実施例１と同様の方法で粒状窒素肥料を作製した後、粒状窒素肥料を熱風乾燥機に入れて、１３０℃で２０分間乾燥した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９７．９％で、収率は５７．８％で粒硬度（圧壊強度）は３．９ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．１％、水分率は０．０％、固結テスト１ヶ月後の固結率は０．０％、固結強度は０．０ｋｇ／ｃｍ２であった。
(Example 3)
After producing granular nitrogenous fertilizer by the same method as Example 1, granular nitrogenous fertilizer was put into a hot air dryer, and it dried at 130 ° C for 20 minutes. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 97.9%, the yield was 57.8%, and the particle hardness (crushing strength) was 3.9 kgf. The granular nitrogen fertilizer is 21.1% ammonia nitrogen, 0.0% moisture content, 0.0% consolidation rate after 1 month consolidation test, and 0.0kg / cm 2 consolidation strength. there were.
（実施例４）
配向度０．９９７の細粒結晶硫安６０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉４０重量部を混合して原料とする以外は、実施例１と同様の方法で粒状窒素肥料を作製した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９８．１％で、収率は６０．５％で粒硬度（圧壊強度）は３．７ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．１％。水分率は０．２％、固結テスト１ヶ月後の固結率は１３．５％、固結強度は０．３ｋｇ／ｃｍ２であった。
Example 4
The same as in Example 1 except that 60 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.997 and 40 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are mixed to obtain a raw material. Granular nitrogen fertilizer was prepared by this method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 98.1%, the yield was 60.5%, and the particle hardness (crushing strength) was 3.7 kgf. Moreover, ammonia nitrogen of granular nitrogen fertilizer is 21.1%. The moisture content was 0.2%, the consolidation rate after 1 month of the consolidation test was 13.5%, and the consolidation strength was 0.3 kg / cm 2 .
（実施例５）
配向度０．９９７の細粒結晶硫安７０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉３０重量部を混合して原料とする以外は、実施例１と同様の方法で粒状窒素肥料を作製した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９８．２％で、収率は６０．１％で粒硬度（圧壊強度）は３．６ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．１％。水分率は０．２％、固結テスト１ヶ月後の固結率は１２．８％、固結強度は０．３ｋｇ／ｃｍ２であった。
(Example 5)
Example 1 except that 70 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.997 and 30 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are used as raw materials. Granular nitrogen fertilizer was prepared by this method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 98.2%, the yield was 60.1%, and the particle hardness (crushing strength) was 3.6 kgf. Moreover, ammonia nitrogen of granular nitrogen fertilizer is 21.1%. The moisture content was 0.2%, the consolidation rate after 1 month of the consolidation test was 12.8%, and the consolidation strength was 0.3 kg / cm 2 .
（実施例６）
配向度０．９９７の細粒結晶硫安８０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉２０重量部を混合して原料とする以外は、実施例１と同様の方法で粒状窒素肥料を作製した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９８．２％で、収率は５９．５％で粒硬度（圧壊強度）は３．４ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．１％。水分率は０．２％、固結テスト１ヶ月後の固結率は１２．１％、固結強度は０．２ｋｇ／ｃｍ２であった。
(Example 6)
Example 1 except that 80 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.997 and 20 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are mixed to obtain a raw material. Granular nitrogen fertilizer was prepared by this method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 98.2%, the yield was 59.5%, and the particle hardness (crushing strength) was 3.4 kgf. Moreover, ammonia nitrogen of granular nitrogen fertilizer is 21.1%. The moisture content was 0.2%, the consolidation rate after 1 month of the consolidation test was 12.1%, and the consolidation strength was 0.2 kg / cm 2 .
（実施例７）
配向度０．９９７の細粒結晶硫安９０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉１０重量部を混合して原料とする以外は、実施例１と同様の方法で粒状窒素肥料を作製した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９８．３％で、収率は５９．１％で粒硬度（圧壊強度）は３．３ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．１％。水分率は０．２％、固結テスト１ヶ月後の固結率は１１．５％、固結強度は０．２ｋｇ／ｃｍ２であった。
(Example 7)
The same as in Example 1 except that 90 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.997 and 10 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are mixed to obtain a raw material. Granular nitrogen fertilizer was prepared by this method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 98.3%, the yield was 59.1%, and the particle hardness (crushing strength) was 3.3 kgf. Moreover, ammonia nitrogen of granular nitrogen fertilizer is 21.1%. The moisture content was 0.2%, the consolidation rate after 1 month of the consolidation test was 11.5%, and the consolidation strength was 0.2 kg / cm 2 .
（実施例８）
配向度０．９９７の細粒結晶硫安６０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉４０重量部を混合して原料とする以外は、実施例２と同様の方法で粒状窒素肥料組成物を作製した。その結果、粒状窒素肥料組成物の２〜４ｍｍ粒径が９７．５％で、収率は５９．２％で粒硬度（圧壊強度）は３．５ｋｇｆであった。また、粒状窒素肥料組成物のアンモニア性窒素は２１．１％で、水分率は０．２％、固結テスト１ヶ月後の固結率は９．５％、固結強度は０．２ｋｇ／ｃｍ２であった。
(Example 8)
Example 2 except that 60 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.997 and 40 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are used as raw materials. A granular nitrogen fertilizer composition was prepared by the method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer composition was 97.5%, the yield was 59.2%, and the particle hardness (crushing strength) was 3.5 kgf. Further, the ammoniacal nitrogen of the granular nitrogen fertilizer composition is 21.1%, the moisture content is 0.2%, the consolidation rate after one month of the consolidation test is 9.5%, and the consolidation strength is 0.2 kg / cm 2 .
（実施例９）
配向度０．９９７の細粒結晶硫安６０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉４０重量部を混合して原料とする以外は、実施例１と同様の方法で粒状肥料組成物を作製した後、粒状窒素肥料を熱風乾燥機に入れて、１３０℃で２０分間乾燥した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９７．１％で、収率は５８．９％で粒硬度（圧壊強度）は４．０ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．１％、水分率は０．０％、固結テスト１ヶ月後の固結率は０．０％、固結強度は０．０ｋｇ／ｃｍ２であった。
Example 9
The same as in Example 1 except that 60 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.997 and 40 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are mixed to obtain a raw material. After producing a granular fertilizer composition by the method, the granular nitrogenous fertilizer was put in a hot air dryer and dried at 130 ° C. for 20 minutes. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 97.1%, the yield was 58.9%, and the particle hardness (crushing strength) was 4.0 kgf. The granular nitrogen fertilizer is 21.1% ammonia nitrogen, 0.0% moisture content, 0.0% consolidation rate after 1 month consolidation test, and 0.0kg / cm 2 consolidation strength. there were.
（実施例１０）
実施例８と同様の方法で粒状窒素肥料組成物を作製した。得られた粒状窒素肥料組成物１００重量部に対して、リン安粒状物６０重量部および塩化カリ粒状物４０重量部を容器に入れて混合し、混合肥料とした。混合肥料の固結テスト１ヶ月後の固結率は０．０％、固結強度は０．０ｋｇ／ｃｍ２であった。
(Example 10)
A granular nitrogen fertilizer composition was prepared in the same manner as in Example 8. With respect to 100 parts by weight of the obtained granular nitrogen fertilizer composition, 60 parts by weight of phosphorous granules and 40 parts by weight of potassium chloride granules were mixed in a container to obtain a mixed fertilizer. The consolidation rate of the mixed fertilizer after one month was 0.0%, and the consolidation strength was 0.0 kg / cm 2 .
（実施例１１）
固結防止材のタルクをベントナイトに変更して実施例５と同様の方法で粒状窒素肥料組成物を作製した。その結果、粒状窒素肥料組成物の２〜４ｍｍ粒径が９２．８％で、収率は２９．０％で粒硬度（圧壊強度）は３．０ｋｇｆであった。また、粒状窒素肥料組成物のアンモニア性窒素は２１．０％、水分率は０．９％、固結テスト１ヶ月後の固結率は４３．５％、固結強度は２．５ｋｇ／ｃｍ２であった。
(Example 11)
A granular nitrogen fertilizer composition was produced in the same manner as in Example 5 except that the anti-caking material talc was changed to bentonite. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer composition was 92.8%, the yield was 29.0%, and the particle hardness (crushing strength) was 3.0 kgf. The granular nitrogen fertilizer composition has an ammoniacal nitrogen content of 21.0%, a moisture content of 0.9%, a consolidation rate after one month of consolidation test of 43.5%, and a consolidation strength of 2.5 kg / cm. 2 .
（比較例１）
配向度０．９９７の細粒結晶硫安５０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉５０重量部を混合して原料とする以外は、実施例１と同様の方法で粒状窒素肥料を作製した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９７．８％で、収率は６０．４％で粒硬度（圧壊強度）は３．４ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．１％。水分率は０．３％、固結テスト１ヶ月後の固結率は１９．５％、固結強度は０．９ｋｇ／ｃｍ２であった。
(Comparative Example 1)
Example 1 except that 50 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.997 and 50 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are used as raw materials. Granular nitrogen fertilizer was prepared by this method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 97.8%, the yield was 60.4%, and the particle hardness (crushing strength) was 3.4 kgf. Moreover, ammonia nitrogen of granular nitrogen fertilizer is 21.1%. The moisture content was 0.3%, the consolidation rate after 1 month of the consolidation test was 19.5%, and the consolidation strength was 0.9 kg / cm 2 .
（比較例２）
配向度０．９８９の細粒結晶硫安６０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉４０重量部を混合して原料とする以外は、実施例１と同様の方法で粒状窒素肥料を作製した。その結果、粒状窒素肥料の２〜４ｍｍ粒径が９８．１％で、収率は６１．０％で粒硬度（圧壊強度）は２．７ｋｇｆであった。また、粒状窒素肥料のアンモニア性窒素は２１．０％、水分率は０．５％、固結テスト１ヶ月後の固結率は７３．０％、固結強度は３．０ｋｇ／ｃｍ２であった。
(Comparative Example 2)
The same as in Example 1 except that 60 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.989 and 40 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are used as raw materials. Granular nitrogen fertilizer was prepared by this method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer was 98.1%, the yield was 61.0%, and the particle hardness (crushing strength) was 2.7 kgf. The granular nitrogen fertilizer is 21.0% ammonia nitrogen, the moisture content is 0.5%, the consolidation rate after one month of consolidation test is 73.0%, and the consolidation strength is 3.0 kg / cm 2 . there were.
（比較例３）
配向度０．９８９の細粒結晶硫安６０重量部と造粒、整粒後にそれぞれ分級を行って得られた篩下微粉４０重量部を混合して原料とする以外は、実施例２と同様の方法で粒状窒素肥料組成物を作製した。その結果、粒状窒素肥料組成物の２〜４ｍｍ粒径が９７．５％で、収率は６０．２％で粒硬度（圧壊強度）は２．５ｋｇｆであった。また、粒状窒素肥料組成物の水分率は０．５％、固結テスト１ヶ月後の固結率は５６．４％、固結強度は２．１ｋｇ／ｃｍ２であった。
(Comparative Example 3)
The same as in Example 2 except that 60 parts by weight of fine crystal ammonium sulfate having an orientation degree of 0.989 and 40 parts by weight of fine powder under sieve obtained by classification after granulation and sizing are mixed to obtain a raw material. A granular nitrogen fertilizer composition was prepared by the method. As a result, the 2-4 mm particle size of the granular nitrogen fertilizer composition was 97.5%, the yield was 60.2%, and the particle hardness (crushing strength) was 2.5 kgf. The moisture content of the granular nitrogen fertilizer composition was 0.5%, the consolidation rate after one month of the consolidation test was 56.4%, and the consolidation strength was 2.1 kg / cm 2 .
以上のように、配向度０．９９５以上の細粒結晶硫安を６０ｗｔ％以上含む細粒結晶硫安を原料とした粒状窒素肥料とすることで、配向度０．９９５未満の細粒結晶硫安を６０ｗｔ％以上の細粒結晶硫安を原料とした粒状窒素肥料と比較して、粒状窒素肥料の粒硬度が高くて粉化率しにくく、水分が低く保管中に固結しにくくすることができた。 As described above, by using a granular nitrogen fertilizer made from fine crystal ammonium sulfate containing 60 wt% or more of fine crystal ammonium sulfate having an orientation degree of 0.995 or more, 60 wt. Of fine crystal ammonium sulfate having an orientation degree of less than 0.995 is used. Compared with a granular nitrogen fertilizer made of more than 1% fine crystalline ammonium sulfate, the granular nitrogen fertilizer has a high particle hardness and is difficult to pulverize, and has a low moisture content and can be hard to solidify during storage.
本発明により、細粒結晶硫安を原料として、粒硬度が高く水分が低いため粉体発生量が少なく、保管中の固結性の低い粒状窒素肥料を得ることができ、肥料としての取り扱いや、機械散布が容易になるとともに、本発明で得られる粒状窒素肥料は、水に溶解するまでの時間も長いため、単肥・混合肥料いずれにおいても、窒素分を効果的に利用することが可能となる。 According to the present invention, using fine crystal ammonium sulfate as a raw material, the amount of powder generated is low because the particle hardness is high and moisture is low, and it is possible to obtain a granular nitrogen fertilizer with low caking properties during storage, handling as a fertilizer, It is easy to spread the machine, and the granular nitrogen fertilizer obtained in the present invention has a long time to dissolve in water, so it is possible to effectively use the nitrogen content in both simple fertilizer and mixed fertilizer. Become.
Claims (15)
１）二次元Ｘ線回折測定において入射Ｘ線の方向と検出器の方向のなす角２θ＝７２．３°における配向度が０．９９５以上である細粒結晶硫安を６０ｗｔ％以上含む原料を造粒して粒状物を得る造粒工程、
２）１）で得られた粒状物を整粒して形状を調節する整粒工程、
３）２）で整粒された粒状物にタルク、ポリエチレングリコール、ステアリン酸金属塩、ラウリル硫酸金属塩、カオリン、炭酸カルシウム、酸化ケイ素、テレフタル酸カルシウム、酸化アルミニウム、酸化チタン、リン酸カルシウム、およびフッ化リチウムから選ばれる少なくとも一種の固結防止材を添加し被覆する被覆工程。 The manufacturing method of the granular nitrogenous fertilizer of Claim 6 containing the following process 1) -3),
1) In a two-dimensional X-ray diffraction measurement, a raw material containing 60 wt% or more of fine crystal ammonium sulfate having an orientation degree of 0.995 or more at an angle 2θ = 72.3 ° between the direction of incident X-rays and the direction of the detector is prepared. Granulation process to obtain granules by granulation,
2) A sizing step of sizing the granular material obtained in 1) to adjust the shape,
3) Talc, polyethylene glycol, metal stearate, metal lauryl sulfate, kaolin, calcium carbonate, silicon oxide, calcium terephthalate, aluminum oxide, titanium oxide, calcium phosphate, and fluoride to the granulated particles in 2) A coating step of adding and coating at least one anti-caking material selected from lithium.
１）二次元Ｘ線回折測定において入射Ｘ線の方向と検出器の方向のなす角２θ＝７２．３°における配向度が０．９９５以上である細粒結晶硫安を６０ｗｔ％以上含む原料を造粒して粒状物を得る造粒工程、
２）１）で得られた粒状物を整粒し形状を調節する整粒工程、
３）２）で整粒された粒状物を乾燥する乾燥工程。 The manufacturing method of the granular nitrogen fertilizer in any one of Claims 1-5 including the following process 1) -3),
1) In a two-dimensional X-ray diffraction measurement, a raw material containing 60 wt% or more of fine crystal ammonium sulfate having an orientation degree of 0.995 or more at an angle 2θ = 72.3 ° between the direction of incident X-rays and the direction of the detector is prepared. Granulation process to obtain granules by granulation,
2) A sizing step of sizing the granular material obtained in 1) to adjust the shape,
3) A drying step of drying the granulated particles in 2).
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| JP2019043797A (en) * | 2017-08-31 | 2019-03-22 | 東レ株式会社 | Granular nk compound fertilizer and method of producing granular nk compound fertilizer |
| JP2020132494A (en) * | 2019-02-22 | 2020-08-31 | 東レ株式会社 | Method of producing granular ammonium sulfate and method of producing granular nitrogen fertilizer |
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| JP2012211047A (en) * | 2011-03-31 | 2012-11-01 | Mitsubishi Chemicals Corp | Method for producing ammonium sulfate |
| JP2013177287A (en) * | 2012-02-02 | 2013-09-09 | Toray Ind Inc | Granulation method for nitrogen fertilizer, method of manufacturing granular nitrogen fertilizer, and granular nitrogen fertilizer |
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| JP2019043797A (en) * | 2017-08-31 | 2019-03-22 | 東レ株式会社 | Granular nk compound fertilizer and method of producing granular nk compound fertilizer |
| JP7013733B2 (en) | 2017-08-31 | 2022-02-15 | 東レ株式会社 | Manufacturing method of granular NK chemical fertilizer and granular NK chemical fertilizer |
| JP2020132494A (en) * | 2019-02-22 | 2020-08-31 | 東レ株式会社 | Method of producing granular ammonium sulfate and method of producing granular nitrogen fertilizer |
| JP7180444B2 (en) | 2019-02-22 | 2022-11-30 | 東レ株式会社 | Method for producing granular ammonium sulfate and method for producing granular nitrogen fertilizer |
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