JP2009215129A - Method of producing resin coated granular fertilizer - Google Patents
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本発明は、樹脂被覆粒状肥料の製造方法に関する。詳しくは、肥料成分の初期溶出が抑制され、肥料成分の溶出が制御された樹脂被覆粒状肥料の製造方法に関する。 The present invention relates to a method for producing a resin-coated granular fertilizer. Specifically, the present invention relates to a method for producing a resin-coated granular fertilizer in which initial elution of fertilizer components is suppressed and elution of fertilizer components is controlled.
近年、農業就労者の高年齢化、就業者数の減少、兼業農家の増加から、より省力型で植物の成長に合わせて肥料成分の溶出が所定の期間持続する肥効調節型樹脂被覆粒状肥料が要求されている。中でも肥料成分の初期溶出が抑制され、肥料成分の溶出が制御された樹脂被覆粒状肥料が望まれている。
肥料成分の溶出を制御するための被膜欠陥の少ない樹脂被覆粒状肥料の製造方法としては、一般に樹脂被膜量を増やして被膜欠陥部分を補修して行く方法が取られている。しかしながらこの方法では、肥料成分量の低下およびコスト高の問題がある。
In recent years, due to the aging of agricultural workers, the decrease in the number of employed workers, and the increase in part-time farmers, it is more labor-saving and the fertilizer effect-type resin-coated granular fertilizer that keeps elution of fertilizer components as the plant grows for a predetermined period Is required. Among them, a resin-coated granular fertilizer in which initial elution of fertilizer components is suppressed and elution of fertilizer components is controlled is desired.
As a method for producing a resin-coated granular fertilizer with few coating defects for controlling the elution of fertilizer components, generally, a method of repairing a coating defect portion by increasing the amount of the resin coating is taken. However, this method has a problem that the amount of the fertilizer component is reduced and the cost is high.
また、被膜欠陥の少ない被覆粒状肥料の製造方法として、粒状肥料の表面を合成樹脂を主成分とする被覆材料で被覆することによって被覆粒状肥料を製造する際に、円形度係数［（４π×粒子の投影面積）／（粒子投影図の輪郭の長さ）２］が０．７以上である粒状肥料を用いる方法が知られている（特許文献１参照）。
しかしながら、肥料成分の溶出性能に与える円形度の影響以上に肥料の種類の影響が大きく、粒状肥料の円形度係数を１に近づけても、必ずしも溶出性能が向上しないという問題を有しおり、肥料成分の初期溶出が少なく、肥料成分の溶出が制御された樹脂被覆粒状肥料を製造する方法が望まれている。
被覆欠陥の少ない被覆粒状肥料のその他の製造方法として、室温下での吸水量が０．０１ｇ−水／ｇ−肥料以上である粒状肥料表面に、鉱産物粉末と室温下で液状のポリオール化合物とを交互にそれぞれ１〜５層被覆することにより、室温下での吸水量を０．００１ｇ−水／ｇ−肥料以上で０．０１ｇ−水／ｇ−肥料未満とした粒状肥料を用いる方法が知られている（特許文献２参照）。
しかしながら、使用するポリオール化合物は比較的粘度が高いため、被覆装置内部への付着が激しく起こり、このため被覆装置内部の清掃が度々必要となり、運転上煩雑であるという問題を有している。
However, the effect of the fertilizer type is more than the influence of the circularity on the elution performance of the fertilizer component, and even if the circularity coefficient of the granular fertilizer is close to 1, the elution performance is not necessarily improved. Therefore, there is a demand for a method for producing a resin-coated granular fertilizer in which the initial elution of the fertilizer is small and the elution of the fertilizer components is controlled.
As another production method of coated granular fertilizer with few coating defects, mineral powder and a polyol compound which is liquid at room temperature on the surface of granular fertilizer having a water absorption amount of 0.01 g-water / g-fertilizer or more at room temperature A method using a granular fertilizer in which water absorption at room temperature is 0.001 g-water / g-fertilizer or more and less than 0.01 g-water / g-fertilizer by coating 1 to 5 layers alternately. (See Patent Document 2).
However, since the polyol compound to be used has a relatively high viscosity, adhesion to the inside of the coating apparatus occurs violently, which necessitates frequent cleaning of the inside of the coating apparatus and has a problem that it is complicated in operation.
本発明は、肥料成分の初期溶出が抑制され、肥料成分の溶出が制御された、すなわち肥料成分の溶出速度が制御され、肥料成分の溶出が所定期間持続する樹脂被覆粒状肥料を製造する方法を提供することにある。 The present invention provides a method for producing a resin-coated granular fertilizer in which initial elution of fertilizer components is suppressed and elution of fertilizer components is controlled, that is, the elution rate of fertilizer components is controlled, and elution of fertilizer components lasts for a predetermined period. It is to provide.
かかる事情下に鑑み、本発明者等は、肥料成分の初期溶出が抑制され、肥料成分の溶出が制御された樹脂被覆粒状肥料の製造方法について鋭意検討した結果、樹脂被膜欠陥は使用する粒状肥料の吸水量の大きいものほど多く、吸水量が小さくなるほど少なくなることを見出し、粒状肥料表面を室温下（２０〜３０℃、以下同じ）で液状の鉱油を添加被覆すれば、被覆装置内部への付着も殆ど無く、その吸水量を容易に小さくすることが可能となり、この方法で粒状肥料の室温下での吸水量を０．０１ｇ−水／ｇ−肥料未満とした後、その表面を樹脂被覆材で被覆処理することによって、肥料成分の初期溶出が抑制され、肥料成分の溶出が制御された樹脂被覆粒状肥料が得られることを見出し、本発明を完成するに至った。 In view of such circumstances, the present inventors have intensively studied a method for producing a resin-coated granular fertilizer in which the initial elution of the fertilizer component is suppressed and the elution of the fertilizer component is controlled. It is found that the larger the water absorption amount is, the smaller the water absorption amount is, and the smaller the water absorption amount is, and if the surface of the granular fertilizer is coated with liquid mineral oil at room temperature (20-30 ° C., the same applies hereinafter), There is almost no adhesion, and it is possible to easily reduce the water absorption amount. After this method, the water absorption amount of the granular fertilizer at room temperature is set to less than 0.01 g-water / g-fertilizer, and then the surface is coated with resin. By carrying out coating treatment with the material, it was found that the initial elution of the fertilizer component was suppressed, and a resin-coated granular fertilizer in which the elution of the fertilizer component was controlled was obtained, and the present invention was completed.
すなわち本発明は、室温下での吸水量が０．００３ｇ−水／ｇ−肥料以上である粒状肥料表面に、室温下で液状の鉱油を添加被覆することにより、室温下での吸水量を０．０1ｇ−水／ｇ−肥料未満とした後、その表面を樹脂被覆材で被覆することを特徴とする樹脂被覆粒状肥料の製造方法である。 That is, according to the present invention, the amount of water absorption at room temperature is reduced to 0 by coating a granular fertilizer surface having a water absorption amount of 0.003 g-water / g-fertilizer or more at room temperature by adding liquid mineral oil at room temperature. A method for producing a resin-coated granular fertilizer, characterized in that the surface is coated with a resin coating material after being less than 0.01 g-water / g-fertilizer.
本発明方法によれば、被覆操作が容易でかつ初期溶出が抑制され、肥料成分の溶出が制御された樹脂被覆粒状肥料を製造することができ、その産業上の利用価値は頗る大きい。 According to the method of the present invention, it is possible to produce a resin-coated granular fertilizer in which coating operation is easy, initial elution is suppressed, and elution of fertilizer components is controlled, and its industrial utility value is very large.
本発明において用いる粒状肥料は、肥料成分を含有する粒状物であり、室温下での吸水量が０．００３ｇ−水／ｇ−肥料以上のものである。
肥料成分は、水稲などの植物栽培において養分を与えるために土壌に施される窒素、リン、カリウム、珪素、マグネシウム、カルシウム、マンガン、ホウ素等の種々の元素を含有する成分であり、粒状肥料の具体例としては、尿素、硝酸アンモニウム、硝酸苦土アンモニウム、塩化アンモニウム、硫酸アンモニウム、リン酸アンモニウム、硝酸ソーダ、硝酸カルシウム、硝酸カリウム、石灰窒素、ホルムアルデヒド加工尿素肥料（ＵＦ）、アセトアルデヒド加工尿素肥料（ＣＤＵ）、イソブチルアルデヒド加工尿素肥料（ＩＢＤＵ）、グアニール尿素（ＧＵ）等の窒素質肥料、過リン酸石灰、重過リン酸石灰、熔成リン肥、腐植酸リン肥、焼成リン肥、重焼リン、苦土過燐酸、ポリリン酸アンモニウム、メタリン酸カリウム、メタリン酸カルシウム、苦土リン酸、硫リン安、リン硝安カリウム、塩リン安等のリン酸質肥料、塩化カリウム、硫酸カリウム、硫酸カリソーダ、硫酸カリ苦土、重炭酸カリウム、リン酸カリウム等のカリウム質肥料、珪酸カルシウム等の珪酸質肥料、硫酸マグネシウム、塩化マグネシウム等のマグネシウム質肥料、生石灰、消石灰、炭酸カルシウム等のカルシウム質肥料、硫酸マンガン、硫酸苦土マンガン、鉱さいマンガン等のマンガン質肥料、ホウ酸、ホウ酸塩等のホウ酸質肥料等の肥料取締法に定められる普通肥料（複合肥料を含む）、および／またはこれらに粒状物の組合せによって得られる窒素―リン酸、窒素―加里、およびリン酸―加里の２成分系、窒素―リン酸―加里の３成分系、あるいはこれらにマグネシウム、マンガン、ホウ素等の植物の生育に必要な要素を含有させた粒状肥料が挙げられる。中でも尿素肥料は常温下での吸水量が通常約０．００５ｇ−水／ｇ−肥料〜０．０１ｇ−水／ｇ−肥料であり、化成肥料等に比較し低い。本発明方法は常温下での吸水量が低い尿素肥料に対し特に好適である。
粒状肥料の粒径は特に限定はないが、製造上の観点から通常１〜１５ｍｍの範囲であり、好ましくは２〜５ｍｍの範囲である。
The granular fertilizer used in the present invention is a granular material containing a fertilizer component, and has a water absorption of 0.003 g-water / g-fertilizer or more at room temperature.
The fertilizer component is a component containing various elements such as nitrogen, phosphorus, potassium, silicon, magnesium, calcium, manganese, and boron that are applied to the soil to provide nutrients in plant cultivation such as paddy rice. Specific examples include urea, ammonium nitrate, ammonium nitrate, ammonium nitrate, ammonium sulfate, ammonium phosphate, sodium nitrate, calcium nitrate, potassium nitrate, lime nitrogen, formaldehyde processed urea fertilizer (UF), acetaldehyde processed urea fertilizer (CDU), Nitrogenous fertilizers such as isobutyraldehyde processed urea fertilizer (IBDU) and guaneaure urea (GU), superphosphate lime, heavy superphosphate lime, molten phosphorus fertilizer, humic phosphate fertilizer, calcined phosphorus fertilizer, heavy calcined phosphorus, bitter Soil perphosphate, ammonium polyphosphate, potassium metaphosphate, calmetaphosphate Phosphoric fertilizers such as humic, bitter phosphate, ammonium sulfate, potassium phosphate, ammonium phosphate, potassium chloride, potassium sulfate, potassium sulfate, potassium sulfate, potassium bicarbonate, potassium phosphate, etc. Fertilizers, siliceous fertilizers such as calcium silicate, magnesium fertilizers such as magnesium sulfate and magnesium chloride, calcium fertilizers such as quick lime, slaked lime and calcium carbonate, manganese fertilizers such as manganese sulfate, sulfated manganese manganese, and mineral manganese, Nitrogen-phosphoric acid, nitrogen-kari, and ordinary fertilizers (including complex fertilizers) defined by the fertilizer control law such as borate fertilizers such as acids and borates, and / or combinations of these Phosphoric acid-Kari two-component system, nitrogen-phosphoric acid-Kari three-component system, or plants such as magnesium, manganese, boron, etc. It includes granular fertilizer which contains the necessary elements for growth. Among them, urea fertilizer usually has a water absorption at room temperature of about 0.005 g-water / g-fertilizer to 0.01 g-water / g-fertilizer, which is lower than that of chemical fertilizer. The method of the present invention is particularly suitable for urea fertilizer having a low water absorption at room temperature.
The particle size of the granular fertilizer is not particularly limited, but is usually in the range of 1 to 15 mm and preferably in the range of 2 to 5 mm from the viewpoint of production.
本発明で使用する鉱油としては、室温下において液状のものであれば良いが、好ましいのは引火点が７０℃以上の危険物第４類第３石油類であり、通常工業用として市販されているものが用いられる。 The mineral oil used in the present invention may be liquid at room temperature, but is preferably a hazardous material class 4 and class 3 petroleum having a flash point of 70 ° C. or higher, and is usually commercially available for industrial use. What is used is used.
室温下で液状の鉱油の添加被覆量は、使用する粒状肥料により一義的ではないが、通常被覆する粒状肥料に対し０．００１重量％〜５重量％である。実施に際しては予備実験により被覆対象となる粒状肥料に鉱油で被覆処理し処理後の吸水量を測定し、所望とする吸水量範囲となる被覆量を簡単に求めることができる。被覆後の肥料の吸水量は０．０１ｇ−水／ｇ−肥料未満、普通には０．００３ｇ−水／ｇ−肥料未満、より好ましくは０．００１ｇ−水／ｇ−肥料未満に調節し得る。被覆処理方法としては特に制限されるものではなく、当該分野で公知の方法が適用し得る。一般的には、転動型の回転円筒や回転皿等の装置で、粒状肥料を転動させながら、これにスプレー添加、混合して被覆する方法が用いられる。 The coating amount of mineral oil that is liquid at room temperature is not unique depending on the granular fertilizer used, but is usually 0.001% to 5% by weight based on the granular fertilizer to be coated. At the time of implementation, the granular fertilizer to be coated can be coated with mineral oil by a preliminary experiment, and the amount of water absorption after the treatment can be measured to easily determine the coating amount within the desired water absorption range. The water absorption of the fertilizer after coating can be adjusted to less than 0.01 g-water / g-fertilizer, usually less than 0.003 g-water / g-fertilizer, more preferably less than 0.001 g-water / g-fertilizer. . The coating method is not particularly limited, and methods known in the art can be applied. Generally, a method of spraying, mixing and coating granular fertilizer while rolling it with an apparatus such as a rolling-type rotating cylinder or rotating dish is used.
前記処理方法で、室温下での吸水量を０．０１ｇ−水／ｇ−肥料未満、好ましくは０．００３ｇ−水／ｇ−肥料未満とした粒状肥料の被覆処理物の表面を被覆処理する樹脂被覆材としては、主に熱硬化性樹脂が使用される。熱硬化性樹脂としては、アルキド樹脂、ウレタン樹脂等が使用され、中でもウレタン樹脂が好ましく用いられる。ウレタン樹脂はポリイソシアネート化合物とポリオール化合物との反応により３次元架橋することにより生成するものである。また、ポリイソシアネート化合物を２種類以上および／またはポリオール化合物を２種類以上混合して用いることもできる。 Resin that coats the surface of a coated product of granular fertilizer having a water absorption amount at room temperature of less than 0.01 g-water / g-fertilizer, preferably less than 0.003 g-water / g-fertilizer in the above treatment method. As the covering material, a thermosetting resin is mainly used. As the thermosetting resin, an alkyd resin, a urethane resin or the like is used, and among them, a urethane resin is preferably used. The urethane resin is produced by three-dimensional crosslinking by a reaction between a polyisocyanate compound and a polyol compound. Further, two or more polyisocyanate compounds and / or two or more polyol compounds can be mixed and used.
ポリイソシアネート化合物としては、例えばトルエンジイソシアネート（以下、ＴＤＩと略称することがある。）、ジフェニルメタンジイソシアネート（ＭＤＩと略称することがある。）、ナフタレンジイソシアネート、トリジンイソシアネート、ヘキサメチレンジイソシアネート、イソホロンジイソシアネート、キシリレンジイソシアネート等を挙げることができ、必要に応じてこれらの混合物を用いることができる。中でも、ＭＤＩ、ＴＤＩまたはこれらから誘導されるオリゴマー体（ポリメリックＭＤＩ、ポリメリックＴＤＩ等）が好適に用いられる。 Examples of the polyisocyanate compound include toluene diisocyanate (hereinafter sometimes abbreviated as TDI), diphenylmethane diisocyanate (sometimes abbreviated as MDI), naphthalene diisocyanate, tolidine isocyanate, hexamethylene diisocyanate, isophorone diisocyanate, xylylene diene. An isocyanate etc. can be mentioned and these mixtures can be used as needed. Among these, MDI, TDI or oligomers derived from these (polymeric MDI, polymeric TDI, etc.) are preferably used.
ポリイソシアネート化合物と反応させるポリオール化合物としては、前記と同様の例えばアミノアルコール、アミン等を開始材として用い、プロピレングリコール、トリメチロールプロパン等の脂肪族アルコールとエチレンオキサイドやプロピレンオキサイドとを重付加して得られるポリエーテルポリオール、テトラヒドロフランを重合して得られるポリテトラメチレンエーテルグリコール等のポリエーテル型ポリオール、イサノ油やひまし油等の水酸基を保有する天然油脂や多価アルコールとポリエーテルポリオールとカルボン酸化合物を反応させる等の方法で得られるポリエステル型ポリオール等が挙げられる。 As the polyol compound to be reacted with the polyisocyanate compound, for example, amino alcohol, amine and the like as described above are used as a starting material, and an aliphatic alcohol such as propylene glycol and trimethylolpropane is polyadded with ethylene oxide and propylene oxide. Polyether polyol obtained, polyether type polyol such as polytetramethylene ether glycol obtained by polymerizing tetrahydrofuran, natural fats and oils possessing hydroxyl groups such as Isano oil and castor oil, polyhydric alcohol, polyether polyol and carboxylic acid compound Examples thereof include polyester-type polyols obtained by a method such as reaction.
使用するポリイソシアネート化合物に由来するＮＣＯ基とポリオール化合物に由来するＯＨ基の当量比、いわゆるＮＣＯ／ＯＨは、通常０．９〜１．２の間で調整される。 The equivalent ratio of the NCO group derived from the polyisocyanate compound to be used and the OH group derived from the polyol compound, so-called NCO / OH, is usually adjusted between 0.9 and 1.2.
ウレタン樹脂原料の硬化促進の目的で添加される触媒としては、例えば、トリエチレンジアミン、Ｎ−メチルモルフォリン、Ｎ，Ｎ−ジメチルモルフォリン、ジアザビシクロウンデセン、イミダゾール、エチルメチルイミダゾール、ジアザビシクロオクタン、２，４，６，−トリス（ジメチルアミノミチル）フェノール等のアミン系触媒、尿素等のアンモニア誘導体、水酸化ナトリウム、水酸化カリウム等のアルカリ性化合物、ジブチルスズラウレート、ジブチルスズマレート等の有機スズ化合物が挙げられる。中でもアミン系触媒が好適に用いられる。これら触媒の量は、ポリイソシアネート化合物とポリオール化合物の総重量に対して、通常、０．０５〜５重量％程度である。 Examples of the catalyst added for the purpose of accelerating the curing of the urethane resin raw material include triethylenediamine, N-methylmorpholine, N, N-dimethylmorpholine, diazabicycloundecene, imidazole, ethylmethylimidazole, diazabicyclo. Amine catalysts such as octane, 2,4,6, -tris (dimethylaminomytyl) phenol, ammonia derivatives such as urea, alkaline compounds such as sodium hydroxide and potassium hydroxide, organic compounds such as dibutyltin laurate and dibutyltin malate A tin compound is mentioned. Of these, amine-based catalysts are preferably used. The amount of these catalysts is usually about 0.05 to 5% by weight based on the total weight of the polyisocyanate compound and the polyol compound.
樹脂被覆材の量は、特に制限されるものではなく、所望する溶出速度、溶出期間に応じて適宜調節される。通常は、粒状肥料に対して３〜１５重量％の範囲内において行なわれる。 The amount of the resin coating material is not particularly limited, and is appropriately adjusted according to a desired elution rate and elution period. Usually, it is performed within a range of 3 to 15% by weight with respect to the granular fertilizer.
樹脂被覆材の被覆処理方法としては特に制限されるものではなく、当該分野で公知の方法が適用し得る。一般的には、温度制御可能な転動型の回転円筒や回転皿等の装置に、前記処理方法で、室温下での吸水量を０．０１ｇ−水／ｇ−肥料未満、好ましくは０．００３ｇ−水／ｇ−肥料未満とした粒状肥料の被覆処理物を供給して転動させながら、これに液状の熱硬化性樹脂を添加被覆し、次いで熱硬化させて被覆処理する方法が用いられる。 The method for coating the resin coating material is not particularly limited, and methods known in the art can be applied. In general, a water-absorbing amount at room temperature is less than 0.01 g-water / g-fertilizer, preferably 0.0. A method is used in which a coating of a granular fertilizer of less than 003 g-water / g-fertilizer is supplied and rolled, and a liquid thermosetting resin is added and coated, followed by thermosetting and coating. .
本発明の方法によって、初期溶出が抑制され、肥料成分の溶出が制御された樹脂被覆粒状肥料が得られる理由は定かでないが、以下のように推察される。
従来の樹脂被覆法では、粒状肥料の細孔の有る部分と無い部分で樹脂の被膜の状態が不均一となる。細孔径が大きく、かつ吸水量の大きい場合には更に被膜の状態が不均一となり、このため被覆量に応じた溶出制御ができなくなると共に、使用する粒状肥料の吸水量が異なる度に、溶出が不安定となり、被覆量に応じた溶出制御が困難になる。
一方、本発明方法では、添加される鉱油が細孔に取込まれて細孔が埋められる。細孔が大きい場合は、添加される鉱油量を増加することにより、細孔が完全に埋められ、結果、極めて細孔の少ない粒状肥料を得ることが出来る。このようにして得られた粒状肥料を樹脂溶液で被覆処理する際には、樹脂溶液は細孔に取込まれることなく被膜を重ねて行くことができることから、被膜厚が均一となり、従って、被覆量に応じた溶出制御が可能になる。
The reason for obtaining a resin-coated granular fertilizer in which initial elution is suppressed and elution of fertilizer components is controlled by the method of the present invention is not clear, but is presumed as follows.
In the conventional resin coating method, the state of the resin coating becomes non-uniform between the portion of the granular fertilizer having pores and the portion having no pores. When the pore size is large and the amount of water absorption is large, the state of the coating is further non-uniform, so that elution control according to the amount of coating becomes impossible, and elution occurs every time the amount of water absorption of the granular fertilizer used differs. It becomes unstable and it becomes difficult to control elution according to the coating amount.
On the other hand, in the method of the present invention, the added mineral oil is taken into the pores to fill the pores. When the pores are large, the amount of mineral oil added is increased to completely fill the pores, and as a result, a granular fertilizer with very few pores can be obtained. When coating the granular fertilizer thus obtained with a resin solution, the resin solution can be layered without being taken into the pores, so that the film thickness becomes uniform, and therefore the coating Elution control according to the amount becomes possible.
以下に実施例を挙げて本発明をさらに具体的に説明するが、本発明はこれら実施例によって何ら限定されるものではない。
なお、実施例中の部および％は特記しない限りすべて重量部および重量百分率を示す。
EXAMPLES Hereinafter, the present invention will be described more specifically with reference to examples, but the present invention is not limited to these examples.
In addition, unless otherwise indicated, all the parts and% in an Example show a weight part and a weight percentage.
また、吸水量および肥料成分の溶出量の測定は以下の方法で行なった。
（１）吸水量の測定：
室温下に、市販のパン型造粒機（容器：ステンレス、容器寸法：２４０ｍｍφ×７５ｍｍ、傾斜角度：４５度、回転数：５０ｒｐｍ）に粒状肥料３００ｇを入れ、転動させながら電動ビュレットを使用し、水を０．０１ｇ／秒の添加速度で、転動する粒状肥料の上部より添加し、粒状肥料が転動しなくなるまで添加し、転動しなくなった時までの水量を測定し、吸水量とした。
（２）肥料成分の溶出量の測定：
複数本の１００ｍｌの栓付きガラス管のそれぞれに、測定する樹脂被覆粒状肥料５ｇを入れ、水１００ｍｌを添加して浸漬し、栓をして２５℃の恒温槽に静置した。
所定期間毎に、ガラス管を恒温槽から取り出し、溶液を化学濾紙で濾過して水中に溶出した肥料成分を定量分析し、溶出量（％）を算出した。
Moreover, the water absorption amount and the elution amount of the fertilizer component were measured by the following methods.
(1) Measurement of water absorption:
At room temperature, put 300g of granular fertilizer into a commercial bread granulator (container: stainless steel, container dimensions: 240mmφ x 75mm, tilt angle: 45 degrees, rotation speed: 50rpm), and use an electric burette while rolling. Add water from the top of the rolling granular fertilizer at an addition rate of 0.01 g / second, add until the granular fertilizer stops rolling, measure the amount of water until it stops rolling, It was.
(2) Measurement of fertilizer component elution amount:
5 g of resin-coated granular fertilizer to be measured was put into each of a plurality of 100 ml glass tubes with stoppers, 100 ml of water was added and immersed, stoppered and placed in a thermostatic bath at 25 ° C.
At predetermined intervals, the glass tube was taken out of the thermostat, the solution was filtered with chemical filter paper, and the fertilizer components eluted in water were quantitatively analyzed, and the elution amount (%) was calculated.
実施例１
（１）室温下での吸水量が、０．００３ｇ-水／ｇ-肥料 未満の粒状肥料の被覆処理物の製造：
室温下において、転動型の被覆装置に粒状化成肥料１６−１６−１６（室温下の吸水量：０．０１８ｇ-水／ｇ-肥料 、平均粒径３．５ｍｍ）（１６−１６−１６はＮ−Ｐ２Ｏ５−Ｋ２Ｏとしての含量％を示す）２０ｋｇを仕込んだ。被覆装置の回転部を２０〜３０ｒｐｍで回転させ、仕込んだ粒状化成肥料を転動状態にした。この転動物の上部から、鉱油（商品名：フッコール コーティングオイル、危険物第４類第３石油類、富士興産株式会社製品）３０９．６ｇ（３６０ｍｌ）をスプレー添加し被覆処理した。得られた被覆処理物の吸水量は０．００２ｇ−水／ｇ−肥料であった。
Example 1
(1) Manufacture of coated processed product of granular fertilizer having a water absorption at room temperature of less than 0.003 g-water / g-fertilizer:
At room temperature, granulated fertilizer 16-16-16 (water absorption amount at room temperature: 0.018 g-water / g-fertilizer, average particle size 3.5 mm) in a rolling type coating device (16-16-16 is 20 kg) (indicating% content as N—P 2 O 5 —K 2 O) was charged. The rotating part of the coating apparatus was rotated at 20 to 30 rpm, and the charged granular fertilizer was put into a rolling state. From the upper part of this animal, 309.6 g (360 ml) of mineral oil (trade name: FUCKOL coating oil, dangerous materials class 4 and 3 petroleum products, manufactured by Fuji Kosan Co., Ltd.) was sprayed and coated. The amount of water absorption of the obtained coated processed product was 0.002 g-water / g-fertilizer.
（２）樹脂被覆粒状肥料の製造：
前記（１）で得た吸水量０．００３ｇ-水／ｇ-肥料 未満の被覆処理物の表面を、以下の方法でウレタン樹脂で被覆して樹脂被覆粒状化成肥料を製造した。被覆処理物に対するウレタン樹脂の被覆量は６％とした。
室温下でポリオール混合槽に分岐ポリエーテルポリオール（スミフェン（商標登録）ＴＭ、住友バイエルウレタン社製）３１２．２ｇと硬化触媒として２，４，６−トリス（ジメチルアミノメチル）フェノール６ｇを加え、３０分撹拌し、混合物３１９．２ｇを得た（以下、混合物Ａと記す。）。
温度制御可能な転動型の被覆装置に被覆処理物１０ｋｇを仕込んだ。被覆装置の回転部を２０〜３０ｒｐｍで回転させ、仕込んだ被覆処理物を転動状態にした。被覆処理物の温度を７０〜７５℃になるまで加熱保持しながら、ポリイソシアネート化合物としてポリメリックＭＤＩ（スミジュール（登録商標）４４Ｖ１０、住友バイエルウレタン社製）２８０．８ｇと混合物Ａ３１９．２ｇを混合して得られる液状の未硬化ウレタン樹脂組成物を除々に添加し熱硬化させながら被覆処理した。この被覆処理に要した時間は約４８分であった。
このようにして得たウレタン樹脂被覆量６％の樹脂被覆粒状化成肥料について、肥料成分溶出性能を測定した。結果を表１に示す。
(2) Production of resin-coated granular fertilizer:
The surface of the coated product having a water absorption of less than 0.003 g-water / g-fertilizer obtained in (1) was coated with a urethane resin by the following method to produce a resin-coated granular fertilizer. The coating amount of the urethane resin with respect to the coated product was 6%.
At room temperature, 312.2 g of branched polyether polyol (Sumiphen (registered trademark) TM, manufactured by Sumitomo Bayer Urethane Co., Ltd.) and 6 g of 2,4,6-tris (dimethylaminomethyl) phenol as a curing catalyst were added to a polyol mixing tank, and 30 The mixture was stirred for 31 minutes to obtain 319.2 g of a mixture (hereinafter referred to as a mixture A).
10 kg of the coated product was charged in a rolling type coating apparatus capable of controlling the temperature. The rotating part of the coating device was rotated at 20 to 30 rpm, and the charged coated product was brought into a rolling state. While maintaining the temperature of the coated product to 70 to 75 ° C., 280.8 g of polymeric MDI (Sumidur (registered trademark) 44V10, manufactured by Sumitomo Bayer Urethane Co., Ltd.) and 319.2 g of the mixture A were mixed as the polyisocyanate compound. The liquid uncured urethane resin composition obtained in this manner was gradually added and coated while being thermally cured. The time required for this coating treatment was about 48 minutes.
With respect to the resin-coated granular fertilizer having a urethane resin coating amount of 6% obtained in this way, the fertilizer component elution performance was measured. The results are shown in Table 1.
比較例１
実施例１で用いたものと同じ粒状化成肥料１６−１６−１６（室温下の吸水量：０．０１８ｇ-水／ｇ-肥料、平均粒径３．５ｍｍ）をそのまま用いて、実施例１と同様にしてウレタン樹脂の被覆量が６％の樹脂被覆粒状化成肥料を製造した。
この樹脂被覆粒状化成肥料について、肥料成分溶出性能を測定した。結果を表１に示す。
Comparative Example 1
The same granular chemical fertilizer 16-16-16 as used in Example 1 (water absorption at room temperature: 0.018 g-water / g-fertilizer, average particle size 3.5 mm) was used as is, and Example 1 Similarly, a resin-coated granular chemical fertilizer with a urethane resin coating amount of 6% was produced.
About this resin-coated granular chemical fertilizer, the fertilizer component elution performance was measured. The results are shown in Table 1.
実施例２
（１）室温下での吸水量が、０．００３ｇ-水／ｇ-肥料 未満の粒状肥料の被覆処理物の製造：
室温下において、転動型の被覆装置に粒状尿素（室温下の吸水量０．００９ｇ−水／ｇ−肥料、平均粒径３．２ｍｍ）２０ｋｇを仕込んだ。被覆装置の回転部を２０〜３０ｒｐｍで回転させ、仕込んだ粒状尿素を転動状態にした。この転動物の上部から、前記の鉱油１５４．８ｇ（１８０ｍｌ）をこの転動物の上部からスプレー添加し被覆処理した。得られた被覆処理物の吸水量は０．００１ｇ−水／ｇ−肥料であった。
Example 2
(1) Manufacture of coated processed product of granular fertilizer having a water absorption at room temperature of less than 0.003 g-water / g-fertilizer:
At room temperature, 20 kg of granular urea (0.009 g of water absorption at room temperature-water / g-fertilizer, average particle diameter of 3.2 mm) was charged in a rolling type coating apparatus. The rotating part of the coating apparatus was rotated at 20 to 30 rpm, and the charged granular urea was brought into a rolling state. From the top of the animal, 154.8 g (180 ml) of the mineral oil was sprayed from the top of the animal and coated. The water absorption of the obtained coated processed product was 0.001 g-water / g-fertilizer.
（２）樹脂被覆粒状肥料の製造：
前記（１）で得た吸水量０．００３ｇ−水／ｇ−肥料未満の被覆処理物の表面を、以下の方法でウレタン樹脂で被覆して樹脂被覆粒状尿素肥料を製造した。被覆処理物に対するウレタン樹脂の被覆量は８％とした。
室温下でポリオール混合槽に分岐ポリエーテルポリオール（スミフェン（商標登録）ＴＭ、住友バイエルウレタン社製）４１７．６ｇと硬化触媒として２，４，６−トリス（ジメチルアミノメチル）フェノール８ｇを加え、３０分撹拌し、混合物４２５．６ｇを得た（以下、混合物Ｂと記す。）。
温度制御可能な転動型の被覆装置に被覆処理物１０ｋｇを仕込んだ。被覆装置の回転部を２０〜３０ｒｐｍで回転させ、仕込んだ被覆処理物を転動状態にした。被覆処理物の温度を７０〜７５℃になるまで加熱保持しながら、ポリイソシアネート化合物としてポリメリックＭＤＩ（スミジュール（登録商標）４４Ｖ１０、住友バイエルウレタン社製）３７４．４ｇと混合物Ｂ４２５．６ｇを混合して得られる液状の未硬化ウレタン樹脂組成物を除々に添加し熱硬化させながら被覆処理した。この被覆処理に要した時間は約６４分であった。
このようにして得たウレタン樹脂被覆量８％の樹脂被覆粒状尿素肥料について、肥料成分溶出性能を測定した。結果を表１に示す。
(2) Production of resin-coated granular fertilizer:
The surface of the coated treated product having a water absorption of less than 0.003 g-water / g-fertilizer obtained in (1) was coated with a urethane resin by the following method to produce a resin-coated granular urea fertilizer. The coating amount of the urethane resin with respect to the coated product was 8%.
At room temperature, 417.6 g of branched polyether polyol (Sumiphen (registered trademark) TM, manufactured by Sumitomo Bayer Urethane Co., Ltd.) and 8 g of 2,4,6-tris (dimethylaminomethyl) phenol as a curing catalyst were added to a polyol mixing tank, and 30 The mixture was stirred for 4 minutes to obtain 425.6 g of a mixture (hereinafter referred to as a mixture B).
10 kg of the coated product was charged in a rolling type coating apparatus capable of controlling the temperature. The rotating part of the coating device was rotated at 20 to 30 rpm, and the charged coated product was brought into a rolling state. While maintaining the temperature of the coated product to 70 to 75 ° C., 374.4 g of polymeric MDI (Sumijoule (registered trademark) 44V10, manufactured by Sumitomo Bayer Urethane Co., Ltd.) as a polyisocyanate compound and 425.6 g of mixture B were mixed. The liquid uncured urethane resin composition obtained in this manner was gradually added and coated while being thermally cured. The time required for this coating treatment was about 64 minutes.
For the resin-coated granular urea fertilizer having a urethane resin coating amount of 8% obtained in this manner, the fertilizer component elution performance was measured. The results are shown in Table 1.
比較例２
実施例２で用いたものと同じ粒状尿素（室温下の吸水量：０．００９ｇ−水／ｇ−肥料、平均粒径３．２ｍｍ）をそのまま用いて、実施例２と同様にしてウレタン樹脂の被覆量が８％の樹脂被覆粒状尿素肥料を製造した。
この樹脂被覆粒状尿素肥料について、肥料成分溶出性能を測定した。結果を表１に示す。
Comparative Example 2
The same granular urea as used in Example 2 (water absorption at room temperature: 0.009 g-water / g-fertilizer, average particle size of 3.2 mm) was used as it was in Example 2 to obtain a urethane resin. A resin-coated granular urea fertilizer with a coating amount of 8% was produced.
About this resin-coated granular urea fertilizer, the fertilizer component elution performance was measured. The results are shown in Table 1.
表１に示すとおり、本発明の方法によって得られた樹脂被覆粒状肥料は、肥料成分の初期溶出が抑制され、肥料成分の溶出が制御されたものとなっている。 As shown in Table 1, in the resin-coated granular fertilizer obtained by the method of the present invention, the initial elution of the fertilizer component is suppressed and the elution of the fertilizer component is controlled.
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| JP2005047725A (en) * | 2003-07-30 | 2005-02-24 | Sumitomo Chemical Co Ltd | Granular fertilizer composition and method of manufacturing the same |
| JP2007290891A (en) * | 2006-04-24 | 2007-11-08 | Sumitomo Chemical Co Ltd | Method for manufacturing resin-coated granular fertilizer |
| JP2008007370A (en) * | 2006-06-29 | 2008-01-17 | Sumitomo Chemical Co Ltd | Coated granular material coated with urethane resin |
| JP2008031012A (en) * | 2006-07-31 | 2008-02-14 | Sumitomo Chemical Co Ltd | Granular material coated with urethane resin |
| JP2008031034A (en) * | 2006-06-29 | 2008-02-14 | Sumitomo Chemical Co Ltd | Biologically active substance-containing coated granular material coated with urethane resin |
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| JP2005047725A (en) * | 2003-07-30 | 2005-02-24 | Sumitomo Chemical Co Ltd | Granular fertilizer composition and method of manufacturing the same |
| JP2007290891A (en) * | 2006-04-24 | 2007-11-08 | Sumitomo Chemical Co Ltd | Method for manufacturing resin-coated granular fertilizer |
| JP2008007370A (en) * | 2006-06-29 | 2008-01-17 | Sumitomo Chemical Co Ltd | Coated granular material coated with urethane resin |
| JP2008031034A (en) * | 2006-06-29 | 2008-02-14 | Sumitomo Chemical Co Ltd | Biologically active substance-containing coated granular material coated with urethane resin |
| JP2008031012A (en) * | 2006-07-31 | 2008-02-14 | Sumitomo Chemical Co Ltd | Granular material coated with urethane resin |
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| JP2012046382A (en) * | 2010-08-27 | 2012-03-08 | Sumitomo Chemical Co Ltd | Method for producing resin-coated granular fertilizer |
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