JP6706899B2 - Coated granular fertilizer - Google Patents
Coated granular fertilizer Download PDFInfo
- Publication number
- JP6706899B2 JP6706899B2 JP2015210847A JP2015210847A JP6706899B2 JP 6706899 B2 JP6706899 B2 JP 6706899B2 JP 2015210847 A JP2015210847 A JP 2015210847A JP 2015210847 A JP2015210847 A JP 2015210847A JP 6706899 B2 JP6706899 B2 JP 6706899B2
- Authority
- JP
- Japan
- Prior art keywords
- water
- granular fertilizer
- coated
- coating layer
- soluble inorganic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000843 powder Substances 0.000 claims description 77
- 239000011247 coating layer Substances 0.000 claims description 63
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- 239000011347 resin Substances 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- -1 inorganic acid salt Chemical class 0.000 claims description 20
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- 239000011591 potassium Substances 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 229910052783 alkali metal Inorganic materials 0.000 claims description 4
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- 150000001342 alkaline earth metals Chemical class 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
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Description
本発明は、樹脂等で粒状肥料を被覆した被覆層表面を親水化処理した被覆粒状肥料に関する。 The present invention relates to a coated granular fertilizer in which the surface of a coating layer coated with a granular fertilizer with a resin or the like is hydrophilized.
溶出の制御、吸湿防止、固結防止、発塵防止等を目的とした、樹脂を含んだ被覆層を有する肥料や農薬等の生物活性物質の被覆粒状物が実用化されている。被覆肥料の使用場面はその用途によって様々であるが、水田や水耕栽培をはじめとして水中で使用される場合も多い。これら被覆肥料は、その被膜の多くに親水性の乏しい樹脂が含まれる。樹脂は一般的に水との親和性に乏しく撥水性が強いため、例えば水田等において用いる際に浮上しやすいと云った性質を有していた。また、畑に施用した場合であっても、潅水や降雨によって土壌表面に露出しやすい傾向があった。 BACKGROUND ART Coated granules of bioactive substances such as fertilizers and pesticides having a coating layer containing a resin have been put into practical use for the purpose of controlling elution, preventing moisture absorption, preventing caking, and preventing dust generation. The use situation of the coated fertilizer varies depending on its use, but it is often used in water such as in paddy fields and hydroponics. Many of these coated fertilizers contain a resin having poor hydrophilicity. Resins generally have a poor affinity with water and strong water repellency, and thus have a property that they easily float when used in, for example, paddy fields. Even when applied to fields, it tended to be exposed on the soil surface due to irrigation and rainfall.
上記の浮上を防止するため、被覆肥料の被膜に親水性を付与する方法が検討されてきた。樹脂を含む被膜に親水性を付与する技術として、界面活性剤を被膜に分散させ更に被膜表面に微粉末を付着させた被覆肥料が開示されている(特許文献1参照)。また被膜の表面に脂肪酸金属塩または脂肪酸金属塩および無機粉体を保持させた被覆肥料(特許文献2参照)、被膜の表面に含水微粉末酸化珪素を付着せしめてなる浮上防止された被覆肥料(特許文献3参照)、被膜の表面に含水無晶形二酸化珪素微粉体を付着させた被覆肥料(特許文献4参照)、被膜の表面に無機微粉と界面活性剤を付着させた被覆肥料(特許文献5参照)、ケイソウ土または含水無定形二酸化珪素微粉末及び界面活性剤を肥料の表面に付着した被覆肥料(特許文献6参照)、ノニオン性界面活性剤を粒子表面に添着させた被覆肥料(特許文献7参照)が開示されている。 In order to prevent the above-mentioned floating, a method of imparting hydrophilicity to the coating film of the coated fertilizer has been studied. As a technique for imparting hydrophilicity to a resin-containing coating, a coated fertilizer in which a surfactant is dispersed in the coating and fine powder is attached to the coating surface is disclosed (see Patent Document 1). Further, a coated fertilizer in which a fatty acid metal salt or a fatty acid metal salt and an inorganic powder are held on the surface of the coating (see Patent Document 2), and a floating fertilizer coated fertilizer in which hydrous fine powder silicon oxide is attached to the surface of the coating ( Patent Reference 3), coated fertilizer in which hydrous amorphous silicon dioxide fine powder is attached to the surface of the coating (see Patent Literature 4), coated fertilizer in which inorganic fine powder and a surfactant are attached to the surface of the coating (Patent Literature 5). ), diatomaceous earth or water-containing amorphous silicon dioxide fine powder and a coated fertilizer having a surfactant attached to the surface of the fertilizer (see Patent Document 6), a coated fertilizer having a nonionic surfactant attached to the particle surface (Patent Document 7) are disclosed.
さらに、強い撥水性を有する被覆肥料の場合に於いても、水田への施肥時に最適の浮上防止効果とその持続性が得られ、しかも被覆肥料の製造時には肥料粒子同士の固結を防止する被覆肥料を得ることのできる、アミノ酸塩類及び/または水溶性高分子化合物で表面を処理した被覆肥料(特許文献8参照)が開示されている。しかしながら、固結防止、発塵防止、浮上防止の3つの機能のうち、1つまたは2つの機能を有することは可能であるが、3つ全ての機能を有するものは存在していなかった。 Furthermore, even in the case of coated fertilizers with strong water repellency, a coating that provides the optimum floating prevention effect and its sustainability when applying it to paddy fields, and prevents the solidification of fertilizer particles during the production of coated fertilizers. A coated fertilizer whose surface is treated with an amino acid salt and/or a water-soluble polymer compound (see Patent Document 8) capable of obtaining a fertilizer is disclosed. However, although it is possible to have one or two functions out of the three functions of caking prevention, dust generation prevention, and floating prevention, none of them have all three functions.
本発明は、一般的に撥水性を示す樹脂を含む被覆層を表面に有する粒状肥料(本明細書において「被覆肥料」と称する。)であって、長期保管後も固結及び発塵を防止し、かつ施用時に水面への浮上を防止できる、すなわち、固結、発塵、浮上を同時に防止できる被覆肥料を提供することを課題とする。 The present invention is a granular fertilizer (hereinafter referred to as "coated fertilizer" in the present specification) having a coating layer containing a resin having water repellency on the surface thereof, and preventing caking and dust generation even after long-term storage. In addition, it is an object of the present invention to provide a coated fertilizer that can prevent floating on the water surface during application, that is, can simultaneously prevent solidification, dust generation, and floating.
前記従来技術の問題点を解決するため鋭意検討した結果、被覆肥料が有する被覆層に、安価で入手が容易である水溶性無機粉体を付着させることにより、被覆層に親水性が賦与されて施用時の水面浮上を防止できる一方、長期保管後の固結および発塵は抑制されるというバランスの取れた作用効果が表れ、上記課題を解決できることを見出し、この知見に基づき本発明を完成するに至った。 As a result of extensive studies to solve the problems of the conventional techniques, the coating layer of the coated fertilizer has a hydrophilic property imparted to the coating layer by attaching a water-soluble inorganic powder which is inexpensive and easily available. While preventing the floating of the water surface at the time of application, it is found that there is a well-balanced function and effect that caking and dust generation after long-term storage are suppressed, and that the above problems can be solved, and the present invention is completed based on this finding. Came to.
本発明は、以下から構成される。
(1)粒状肥料表面に樹脂を含む被覆層を有し、該被覆層の表面に水溶性無機粉体が保持された、被覆粒状肥料。
(2)上記水溶性無機粉体の割合が、粒状肥料表面に樹脂を含む被覆層を有する被覆肥料100重量部に対して0.01〜1.0重量部である、(1)に記載の被覆粒状肥料。
(3)上記水溶性無機粉体の粒径が0.1〜150μmである、(1)または(2)に記載の被覆粒状肥料。
(4)上記水溶性無機粉体がアルカリ金属またはアルカリ土類金属の無機酸塩またはハロゲン化物である、(1)〜(3)のいずれか1項に記載の被覆粒状肥料。
(5)上記水溶性無機粉体がカリウムの無機酸塩またはハロゲン化物である、(4)に記載の被覆粒状肥料。
The present invention consists of the following.
(1) A coated granular fertilizer having a coating layer containing a resin on the surface of the granular fertilizer, and the water-soluble inorganic powder retained on the surface of the coating layer.
(2) The ratio of the water-soluble inorganic powder is 0.01 to 1.0 parts by weight with respect to 100 parts by weight of the coated fertilizer having a coating layer containing a resin on the surface of the granular fertilizer. Coated granular fertilizer.
(3) The coated granular fertilizer according to (1) or (2), wherein the water-soluble inorganic powder has a particle size of 0.1 to 150 μm.
(4) The coated granular fertilizer according to any one of (1) to (3), wherein the water-soluble inorganic powder is an alkali metal or alkaline earth metal inorganic acid salt or halide.
(5) The coated granular fertilizer according to (4), wherein the water-soluble inorganic powder is an inorganic acid salt or halide of potassium.
本発明の被覆粒状肥料は、施用時に水面への浮上を防止し、更に長期保管後も浮上防止効果と固結および発塵防止効果とが両立する有用な被覆粒状肥料である。なお、本発明により防止することのできる「固結」とは、肥料の粒同士が付着している状態であり、木槌で叩く等の強い力を加えても崩壊しない状態だけでなく、手で触れる等の弱い力を加えることで崩壊する状態も含むものとする。 The coated granular fertilizer of the present invention is a useful coated granular fertilizer that prevents floating on the water surface during application and has both the floating prevention effect and the consolidation and dust generation prevention effect even after long-term storage. The "caking" that can be prevented by the present invention is a state in which the fertilizer grains are attached to each other, and not only the state in which they do not collapse even when a strong force such as hitting with a mallet is applied, It also includes the state of collapse by applying a weak force such as touching.
本発明に係る被覆粒状肥料は基本的に、芯材となる粒状肥料と、当該粒状肥料の表面を被覆する樹脂を含む被覆層と、当該被覆層の表面に保持された水溶性無機粉体とにより構成される。 The coated granular fertilizer according to the present invention is basically a granular fertilizer serving as a core material, a coating layer containing a resin coating the surface of the granular fertilizer, and a water-soluble inorganic powder retained on the surface of the coating layer. It is composed of
「水溶性無機粉体」とは水溶性の無機化合物の粉体である。水溶性は、所定の温度で水に対して一定量溶解する性質を表し、無機化合物粉体を被覆層の表面に保持させたときに本発明の作用効果が奏される限り、その性質の度合い特に限定されるものではない。水溶性無機粉体の25℃の水に対する溶解度は、好ましくは1.0〜50.0重量%(g/mL)であり、さらに好ましくは10.0〜40.0重量%である。 The "water-soluble inorganic powder" is powder of a water-soluble inorganic compound. Water solubility represents a property of dissolving a certain amount in water at a predetermined temperature, and as long as the effect of the present invention is exhibited when the inorganic compound powder is held on the surface of the coating layer, the degree of the property. It is not particularly limited. The solubility of the water-soluble inorganic powder in water at 25°C is preferably 1.0 to 50.0% by weight (g/mL), and more preferably 10.0 to 40.0% by weight.
水溶性の無機化合物としては、アルカリ金属またはアルカリ土類金属の無機酸塩(炭酸塩、硫酸塩、ケイ酸塩、リン酸塩等)またはハロゲン化物(塩化物等)が好ましい。このような水溶性の無機化合物の微粉体を保持させることで、浮上防止効果と固結防止効果を両立させることができる。 As the water-soluble inorganic compound, an inorganic acid salt (carbonate, sulfate, silicate, phosphate, etc.) or a halide (chloride, etc.) of an alkali metal or an alkaline earth metal is preferable. By holding such a fine powder of a water-soluble inorganic compound, it is possible to achieve both the floating prevention effect and the caking prevention effect.
特に、カリウムの無機酸塩またはハロゲン化物は吸湿性が低いので好ましい。このようなカリウム化合物の中でも、塩化カリウムまたは硫酸カリウムは、吸湿後べたつきが発生しにくく固結原因になりにくいため好ましく、吸湿性のより低い硫酸カリウムがさらに好ましい。 Particularly, inorganic acid salts or halides of potassium are preferable because they have low hygroscopicity. Among these potassium compounds, potassium chloride or potassium sulfate is preferable because it is less likely to cause stickiness after moisture absorption and is unlikely to cause caking, and potassium sulfate having lower hygroscopicity is more preferable.
本発明で用いる水溶性無機化合物は粉体である。水溶性無機粉体の粒径は0.1〜150μmが好ましく、1〜25μmがより好ましい。粒径がこの範囲であれば、被覆層の表面に保持されやすく(付着性が良く)、親水性も優れているため、浮上防止効果を発現しやすい。このような粒径を有する水溶性無機粉体は、適切な目開きを有する篩を用いた篩分により得られる。例えば、目開きが25μmの篩を通過した水溶性無機粉体は、粒径が25μm未満(通常1μm以上)である水溶性無機粉体であるとみなすことができる。 The water-soluble inorganic compound used in the present invention is a powder. The particle diameter of the water-soluble inorganic powder is preferably 0.1 to 150 μm, more preferably 1 to 25 μm. When the particle size is in this range, the particles are easily retained on the surface of the coating layer (having good adhesion) and have excellent hydrophilicity, so that the effect of preventing floating is easily exhibited. The water-soluble inorganic powder having such a particle size can be obtained by sieving using a sieve having an appropriate mesh size. For example, a water-soluble inorganic powder that has passed through a sieve having an opening of 25 μm can be regarded as a water-soluble inorganic powder having a particle size of less than 25 μm (usually 1 μm or more).
水溶性無機粉体の粒径が適切であれば、その保持量が多いほど浮上防止効果は高まるが、水溶性無機粉体も剥離しやすくなるために、被覆粒状肥料取り扱い時の粉塵の発生量が多くなる。そのため、被覆層の表面に保持させる水溶性無機粉体は、浮上防止効果の観点からは被覆肥料100重量部に対して0.01重量部以上の割合が好ましいが、それと同時に発塵防止効果も満足させる観点からは、被覆肥料100重量部に対して0.01〜1.0重量部の割合が好ましく、0.05〜1.0重量部の割合がより好ましい。水溶性無機粉体の保持量は、後記実施例に示すように、被覆粒状肥料を水に浸漬したときに溶解した水溶性無機粉体を定量することによって正確に把握することができる。被覆肥料の被覆層表面に水溶性無機粉体を付着させる処理(表面処理)における水溶性無機粉体の「添加量」のほぼ全量が、上記「保持量」となるように調節することが好ましい。 If the particle size of the water-soluble inorganic powder is appropriate, the higher the retention amount is, the higher the anti-floating effect will be, but the water-soluble inorganic powder will also easily peel off, so the amount of dust generated when handling coated granular fertilizer Will increase. Therefore, the water-soluble inorganic powder to be retained on the surface of the coating layer is preferably 0.01 part by weight or more based on 100 parts by weight of the coated fertilizer from the viewpoint of the floating prevention effect, but at the same time, the dust generation prevention effect From the viewpoint of satisfying it, the proportion of 0.01 to 1.0 parts by weight is preferable, and the proportion of 0.05 to 1.0 parts by weight is more preferable, relative to 100 parts by weight of the coated fertilizer. The retained amount of the water-soluble inorganic powder can be accurately grasped by quantifying the water-soluble inorganic powder dissolved when the coated granular fertilizer is immersed in water, as shown in Examples below. It is preferable to adjust so that almost all of the "addition amount" of the water-soluble inorganic powder in the treatment (surface treatment) for attaching the water-soluble inorganic powder to the coating layer surface of the coated fertilizer becomes the "retention amount". ..
本発明では本質的に、水溶性無機粉体を被覆層表面に保持させることにより、前述したような固結、発塵、浮上を同時に防止することができる。しかしながら必要に応じて、本発明の効果を損なわない範囲で、デンプン等の多糖類、シリカや含水無晶形二酸化珪素等の非水溶性無機粉体、脂肪族金属塩等、従来の被覆肥料の被覆層の表面に保持(付着)させていた物質を水溶性無機粉体と併用してもかまわない。 In the present invention, essentially, by holding the water-soluble inorganic powder on the surface of the coating layer, it is possible to simultaneously prevent the above-mentioned solidification, dust generation, and floating. However, if necessary, to the extent that the effects of the present invention are not impaired, polysaccharides such as starch, non-water-soluble inorganic powders such as silica and hydrous amorphous silicon dioxide, aliphatic metal salts, etc. The substance retained (attached) on the surface of the layer may be used together with the water-soluble inorganic powder.
本発明における浮上防止効果は、粒状肥料を被覆した樹脂を含有する疎水性の被覆層表面に水溶性無機粉体を付着させて、表面を親水性にすることで得られる。一方、粒状肥料(被覆肥料)は水分の存在により固結が発生するので、製造後から長期保管時に固結を防止するためには、被覆層表面の保持させる水溶性無機粉体は吸湿性が少ないことが好ましい。 The effect of preventing floating in the present invention is obtained by making the surface hydrophilic by adhering a water-soluble inorganic powder to the surface of a hydrophobic coating layer containing a resin coated with granular fertilizer. On the other hand, granular fertilizer (coated fertilizer) causes solidification due to the presence of water. Therefore, in order to prevent solidification during long-term storage after production, the water-soluble inorganic powder held on the surface of the coating layer has hygroscopicity. It is preferably small.
ちなみに、水溶性無機化合物と水溶性有機化合物の吸湿性を比較すると、一般に水溶性有機化合物の吸湿性が高く、水溶性無機化合物の吸湿性は低い。よって、本発明では水溶性有機化合物ではなく水溶性無機化合物を用いることで、固結防止効果が得られるようにしている。 By the way, when comparing the hygroscopicity of the water-soluble inorganic compound and the water-soluble organic compound, the hygroscopicity of the water-soluble organic compound is generally high and the hygroscopicity of the water-soluble inorganic compound is low. Therefore, in the present invention, the solidification preventing effect is obtained by using the water-soluble inorganic compound instead of the water-soluble organic compound.
被覆層の表面に水溶性無機粉体を保持させる方法は特に限定されないが、公知の混合器、例えば転動ドラム、パン、ポットミキサー等のような粒子を転動させる装置を用い、被覆肥料を転動させながら水溶性無機粉体を添加し、被覆層に付着させる方法が挙げられる。付着処理時の温度等の条件は特に限定されるものではないが、付着を効率よく行うために、被覆層の融着等が起こらず、被覆肥料の溶出挙動等の品質に影響のない範囲で被覆層の表面温度を上げる等、水溶性無機粉体の被覆層への付着性に関係する条件を制御することが推奨される。 The method for holding the water-soluble inorganic powder on the surface of the coating layer is not particularly limited, but a known mixer, for example, a rolling drum, a pan, a device for rolling particles such as a pot mixer, is used to coat the fertilizer. A method of adding a water-soluble inorganic powder while rolling and adhering it to the coating layer can be mentioned. Conditions such as the temperature during the adhesion treatment are not particularly limited, but in order to perform the adhesion efficiently, fusion of the coating layer does not occur, and within the range that does not affect the quality such as the elution behavior of the coated fertilizer. It is recommended to control the conditions related to the adhesion of the water-soluble inorganic powder to the coating layer, such as raising the surface temperature of the coating layer.
本発明における粒状肥料としては窒素質肥料、燐酸質肥料、加里質肥料のほか、植物必須要素のカルシウム、マグネシウム、硫黄、鉄、微量要素やケイ素等を含有する肥料を挙げることができる。窒素質肥料の例としては硫酸アンモニア、尿素、硝酸アンモニアのほか、イソブチルアルデヒド縮合尿素、アセトアルデヒド縮合尿素が挙げられる。燐酸質肥料の例としては過燐酸石灰、熔成リン肥、焼成リン肥が挙げられる。加里質肥料の例としては硫酸加里、塩化加里、ケイ酸加里肥料が挙げられる。肥料の形態としては特に限定されない。また、肥料の三要素(窒素、りん酸、加里)の合計成分量が30%以上の高度化成肥料や配合肥料、更には有機質肥料でもよい。また硝酸化成抑制材や農薬を含む肥料でもよい。 Examples of the granular fertilizer in the present invention include nitrogenous fertilizers, phosphate fertilizers, potassium fertilizers, and fertilizers containing essential plant elements such as calcium, magnesium, sulfur, iron, trace elements and silicon. Examples of nitrogenous fertilizers include ammonia sulfate, urea, and ammonium nitrate, as well as isobutyraldehyde condensed urea and acetaldehyde condensed urea. Examples of the phosphate fertilizer include lime superphosphate, fused phosphorus fertilizer, and calcined phosphorus fertilizer. Examples of potassium fertilizers include potassium sulfate, chloride chloride, and silica silicate fertilizer. The form of fertilizer is not particularly limited. Further, advanced chemical fertilizers and compound fertilizers having a total content of the three components of fertilizers (nitrogen, phosphoric acid, potassium) of 30% or more, and further organic fertilizers may be used. Further, a fertilizer containing a nitrification inhibitor or a pesticide may be used.
粒状肥料の造粒方法としては、押出造粒法、流動層式造粒法、転動造粒法、圧縮造粒法、被覆造粒法、吸着造粒法等を用いることができる。本発明においてはこれらの造粒法の何れを使用してもよい。 As a granulation method for the granular fertilizer, an extrusion granulation method, a fluidized bed granulation method, a tumbling granulation method, a compression granulation method, a coating granulation method, an adsorption granulation method, or the like can be used. Any of these granulation methods may be used in the present invention.
本発明に用いられる被覆肥料の粒子径は特に限定されるものではないが、1.0〜10.0mmであることが好ましい。より好ましくは2.0〜4.0mmが90重量%以上含むものであり、これらはふるい目開きを調節することで容易に取得できる。 The particle size of the coated fertilizer used in the present invention is not particularly limited, but it is preferably 1.0 to 10.0 mm. More preferably, 2.0 to 4.0 mm contains 90% by weight or more, and these can be easily obtained by adjusting the sieve opening.
本発明の被覆粒状肥料の被覆層は、従来の被覆肥料と同様、粒状肥料表面を被覆し、肥料成分を徐々に溶出させる(つまり徐放性を賦与する)機能を有する。被覆層に用いることのできる樹脂は特に限定されるものではなく、熱可塑性樹脂及び熱硬化性樹脂の何れであってもよい。中でも環境保全の点で光崩壊性樹脂や生分解性樹脂を用いるか、それらを配合した樹脂組成物を用いるのが好ましい。 Like the conventional coated fertilizer, the coating layer of the coated granular fertilizer of the present invention has a function of coating the surface of the granular fertilizer and gradually eluting the fertilizer component (that is, imparting the sustained release property). The resin that can be used for the coating layer is not particularly limited, and may be either a thermoplastic resin or a thermosetting resin. Above all, from the viewpoint of environmental protection, it is preferable to use a photodegradable resin or a biodegradable resin, or to use a resin composition containing them.
熱可塑性樹脂の例としてはオレフィン系重合体、塩化ビニリデン系重合体、ジエン系重合体、ワックス類、ポリエステル、石油樹脂、天然樹脂、油脂及びその変性物を挙げることができる。 Examples of thermoplastic resins include olefin polymers, vinylidene chloride polymers, diene polymers, waxes, polyesters, petroleum resins, natural resins, fats and oils and modified products thereof.
オレフィン系重合体としては、低密度ポリエチレン(密度0.88〜0.93g/cm3)、高密度ポリエチレン(密度0.94〜0.97g/cm3)、直鎖状低密度ポリエチレン、超低密度ポリエチレン、エチレン−酢酸ビニル共重合体(酢酸ビニル含有量1〜40重量%)、及びエチレン−α−オレフィン共重合体(密度0.88〜0.94g/cm3)、ポリプロピレン、エチレン−ポリプロピレン共重合体、エチレン−ブタジエン共重合体、エチレン−一酸化炭素共重合体、エチレン−ヘキセン共重合体、ポリブテン、ブテン−エチレン共重合体、ブテン−プロピレン共重合体、ポリスチレン、エチレン−酢酸ビニル−一酸化炭素共重合体、エチレン−アクリル酸共重合体、エチレン−メタアクリル酸共重合体及びエチレン−メタアクリル酸エステル共重合体が例示できる。塩化ビニリデン系重合体としては、塩化ビニリデン−塩化ビニル共重合体、ジエン系重合体の水素化物が例示できる。尚、上記の樹脂はメルトフローレートや分子量、分子量分布、使用触媒、製造プロセス等は特に限定されるものではない。 As the olefin polymer, low density polyethylene (density 0.88 to 0.93 g/cm 3 ), high density polyethylene (density 0.94 to 0.97 g/cm 3 ), linear low density polyethylene, ultra low Density polyethylene, ethylene-vinyl acetate copolymer (vinyl acetate content 1-40% by weight), and ethylene-α-olefin copolymer (density 0.88-0.94 g/cm 3 ), polypropylene, ethylene-polypropylene Copolymer, ethylene-butadiene copolymer, ethylene-carbon monoxide copolymer, ethylene-hexene copolymer, polybutene, butene-ethylene copolymer, butene-propylene copolymer, polystyrene, ethylene-vinyl acetate- Examples thereof include carbon monoxide copolymers, ethylene-acrylic acid copolymers, ethylene-methacrylic acid copolymers and ethylene-methacrylic acid ester copolymers. Examples of vinylidene chloride-based polymers include vinylidene chloride-vinyl chloride copolymers and hydrides of diene-based polymers. The melt flow rate, the molecular weight, the molecular weight distribution, the catalyst used, the manufacturing process, etc. of the above resin are not particularly limited.
ジエン系重合体としてはブタジエン重合体、イソプレン重合体、クロロプレン重合体、ブタジエン−スチレン共重合体、EPDM重合体、スチレン−イソプレン共重合体等またはブタジエン−エチレン−メタクリル酸共重合体等の3元共重合物が例示できる。 As the diene polymer, a terpolymer such as a butadiene polymer, an isoprene polymer, a chloroprene polymer, a butadiene-styrene copolymer, an EPDM polymer, a styrene-isoprene copolymer, or a butadiene-ethylene-methacrylic acid copolymer is used. A copolymer can be illustrated.
ワックス類としては密ロウ、木ロウ、パラフィン、ポリエチレンワックス等が例示でき、ポリエステルとしてはポリ乳酸、ポリカプロラクトン等の脂肪族ポリエステルやポリエチレンテレフタレート等の芳香族ポリエステルが例示でき、天然樹脂としては天然ゴム、ロジン等が例示でき、油脂及びその変性物としては硬化物、固形脂肪酸及び金属塩等が例示できる。 Examples of waxes include beeswax, wood wax, paraffin, and polyethylene wax, examples of polyester include aliphatic polyesters such as polylactic acid and polycaprolactone, and aromatic polyesters such as polyethylene terephthalate, and examples of natural resins include natural rubber. , Rosin and the like, and examples of fats and oils and modified products thereof include hardened products, solid fatty acids and metal salts.
熱硬化性樹脂としてはフェノール樹脂、アルキド樹脂、不飽和ポリエステル、エポキシ樹脂、ケイ素樹脂、ウレタン樹脂及び乾性油等を挙げることができる。これらの熱硬化性樹脂は数多くのモノマーの組み合わせが有るが、本発明においてはモノマーの種類や組み合わせは限定されるものではない。またモノマー同士の重合物の他に、2量体またはポリマー化したもの、またはその混合物の重合物であっても良い。また種類の異なる複数の樹脂を配合したものであってもよい。 Examples of the thermosetting resin include phenol resin, alkyd resin, unsaturated polyester, epoxy resin, silicon resin, urethane resin and drying oil. These thermosetting resins have many combinations of monomers, but the types and combinations of the monomers are not limited in the present invention. In addition to a polymer of monomers, a polymer of a dimer or a polymer, or a mixture thereof may be used. It may also be a mixture of a plurality of different types of resins.
被覆粒状肥料の被覆層には任意で、フィラーとして、タルク、マイカ、セリタイト、ガラスフレーク、各種金属箔、黒鉛、BN(六方晶)、MIO(板状酸化鉄)、板状炭酸カルシウム、板状水酸化アルミニウム等の板状フィラー;炭酸カルシウム、シリカ、クレー、各種鉱石粉砕品、澱粉等の球状フィラー;硫黄等を添加することができる。 As a filler in the coating layer of coated granular fertilizer, talc, mica, seritite, glass flakes, various metal foils, graphite, BN (hexagonal), MIO (plate iron oxide), plate calcium carbonate, plate Plate-like filler such as aluminum hydroxide; spherical filler such as calcium carbonate, silica, clay, various ore crushed products, starch and the like; sulfur and the like can be added.
被覆層がフィラーを含む場合、その含有割合は特に限定されるものではないが、樹脂に対して5〜90重量部が好ましく、20〜60重量部がより好ましい。 When the coating layer contains a filler, the content ratio thereof is not particularly limited, but is preferably 5 to 90 parts by weight, and more preferably 20 to 60 parts by weight with respect to the resin.
被覆粒状肥料の被覆層には任意で、界面活性剤として、ポリオールの脂肪酸エステルに代表されるノニオン界面活性剤、非イオン系界面活性剤等を添加することができる。被覆層が界面活性剤を含む場合、その含有割合は特に限定されるものではないが、樹脂に対して0.01〜10重量部が好ましく、0.1〜5重量部がより好ましい。 The coating layer of the coated granular fertilizer may optionally contain, as a surfactant, a nonionic surfactant represented by a fatty acid ester of polyol, a nonionic surfactant, or the like. When the coating layer contains a surfactant, the content ratio thereof is not particularly limited, but is preferably 0.01 to 10 parts by weight, and more preferably 0.1 to 5 parts by weight with respect to the resin.
被覆粒状肥料の被覆層には任意で、被覆層に含まれる樹脂を分解させるため、種々の有機金属化合物を添加してもよい。有機金属化合物としては、例えば有機金属錯体や有機酸金属塩等が挙げられる。中でも光分解性の調節が容易なことから、鉄錯体やカルボン酸鉄が好ましい。例えば鉄錯体としては鉄アセチルアセトナート、鉄アセトニルアセトネート、鉄のジアルキルジチオカルバメート、ジチオホスフェート、キサンテート、及びベンズチアゾール等が挙げられる。カルボン酸鉄としてはカプリル酸、カプリン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、イソステアリン酸、ベヘン酸、オレイン酸、リノール酸、リノレン酸等の鉄化合物が挙げられる。これらは単独で添加してもよいし、2種以上を組み合わせて添加してもよい。被覆層中の有機金属化合物の割合は、0.0001〜1重量部が好ましく、より好ましくは0.001〜0.5重量部である。上記の割合であれば、被覆粒状肥料の使用後には崩壊性または分解性が得られ、保管中には当初の品質が維持される。 Various organometallic compounds may optionally be added to the coating layer of the coated granular fertilizer in order to decompose the resin contained in the coating layer. Examples of the organic metal compound include organic metal complexes and organic acid metal salts. Of these, iron complexes and iron carboxylates are preferable because their photodegradability can be easily adjusted. Examples of the iron complex include iron acetylacetonate, iron acetonyl acetonate, iron dialkyldithiocarbamate, dithiophosphate, xanthate, and benzthiazole. Examples of iron carboxylates include iron compounds such as caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, isostearic acid, behenic acid, oleic acid, linoleic acid, and linolenic acid. These may be added alone or in combination of two or more. The proportion of the organometallic compound in the coating layer is preferably 0.0001 to 1 part by weight, more preferably 0.001 to 0.5 part by weight. With the above proportion, disintegration or degradability is obtained after using the coated granular fertilizer, and the initial quality is maintained during storage.
被覆肥料の製造方法、すなわち粒状肥料の表面に被覆層を形成させる方法は、特に限定されるものではない。例えば、溶融させた樹脂及び必要に応じて用いられる上述したような添加物(樹脂等という)を粒状肥料表面に噴霧する方法、溶剤に樹脂等を溶解または懸濁させた溶液またはエマルジョンを粒状肥料表面に噴霧する方法(以下「溶解液噴霧法」という)、樹脂等の粉末を粒状肥料表面に付着させ、その後溶融して被膜を形成させる方法、モノマーを粒状肥料表面に噴霧し、表面で反応させて樹脂化(被膜化)する方法、更に樹脂等の溶融液または溶解液に粒状肥料を浸すディップ法等で製造することができる。 The method for producing the coated fertilizer, that is, the method for forming the coating layer on the surface of the granular fertilizer is not particularly limited. For example, a method of spraying a molten resin and the above-described additives (which are referred to as resins, etc.) used as necessary on the surface of the granular fertilizer, a solution or emulsion in which the resin or the like is dissolved or suspended in a solvent is used as the granular fertilizer Method of spraying on the surface (hereinafter referred to as "solution spray method"), method of adhering powder such as resin on the surface of granular fertilizer, then melting to form a film, spraying monomer on the surface of granular fertilizer, and reacting on the surface It can be produced by a method of making it into a resin (coating), and a dipping method in which granular fertilizer is dipped in a melt or a solution of a resin or the like.
被覆層の厚さは樹脂等の種類や組成、粒状肥料の大きさ、意図する肥料成分の溶出パターンによって適宜選択可能であるが、平均で10〜100μmが好ましく、20〜70μmがより好ましい。また被覆層の被覆率(被覆肥料に対する被覆層の重量の割合)は、1〜20重量部が好ましく、2〜15重量部がより好ましい。 The thickness of the coating layer can be appropriately selected depending on the type and composition of the resin and the like, the size of the granular fertilizer, and the elution pattern of the intended fertilizer component, but it is preferably 10 to 100 μm on average, and more preferably 20 to 70 μm. The coating rate of the coating layer (ratio of the weight of the coating layer to the coated fertilizer) is preferably 1 to 20 parts by weight, more preferably 2 to 15 parts by weight.
以下、実施例によって本発明を説明するが、本発明はこれらにより限定されるものではない。 Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited thereto.
1.被覆肥料の作製
図1に示す製造装置を用いて、次の方法により粒状尿素の表面に被覆層を形成した。製造装置内では、熱風が流動層1の下部から上部に向けて流れ集塵機6を通過し、コンデンサー7でガスを冷却し、溶媒を凝縮回収する。コンデンサー7を通過したガスはブロワー8からヒーター12を通過して加熱され熱風として再度流動層1へ導かれるように循環している。このようなクローズドシステムを採用することで溶媒を外部に排出することはない。
1. Production of Coated Fertilizer Using the production apparatus shown in FIG. 1, a coating layer was formed on the surface of granular urea by the following method. In the manufacturing apparatus, hot air flows from the lower part to the upper part of the fluidized bed 1 and passes through the
粒子3として粒状尿素(粒子径2.0〜4.0mm、平均粒径3.0mm)15kgを流動層1の側面に設置されている投入口から投入し、流動層1下部より導入される熱風および流動層1底部に設置される攪拌浴で流動状態にした。この際、粒子温度が60±2℃になるように、熱風流量及び熱風温度を調節した。熱風流量はブロワー9と流動層1の間に設置した流量計で測定しながら調節し、熱風温度は粒子温度や排気温度(流動層1上部温度)を測定しながら調節した。
As the
他方、溶解槽9に被覆層の組成としてポリエチレン(低密度ポリエチレン、密度0.923g/cm3(JIS K 6760)、メルトフローレート(MFR)0.3g/10min.(JIS K 6760))50重量部、コーンスターチ5重量部、タルク(平均粒径10μm)45重量部、ステアリン酸鉄0.01重量部の各成分とテトラクロロエチレン1900重量部を投入し、100±2℃で30分間混合撹拌することによって樹脂を溶解し、濃度5重量%の均一な噴霧液5を調製した。被覆が終了するまで溶解槽9は常時攪拌した。
On the other hand, polyethylene (low density polyethylene, density 0.923 g/cm 3 (JIS K 6760), melt flow rate (MFR) 0.3 g/10 min. (JIS K 6760)) 50 weight as the composition of the coating layer in the dissolution tank 9. Parts, 5 parts by weight of corn starch, 45 parts by weight of talc (
噴霧液5を流動層1の上部に設置されているスプレーノズル2に流速約110kg/hで輸送し、流動中の粒状尿素に噴霧し吹き付けた。吹き付けられた噴霧液に含まれるテトラクロロエチレンはコンデンサー7により凝縮・回収されてタンク11で貯蔵され、溶解槽9へ導かれる。
The spray liquid 5 was transported to the spray nozzle 2 installed in the upper part of the fluidized bed 1 at a flow rate of about 110 kg/h, and sprayed on the flowing granular urea. Tetrachloroethylene contained in the sprayed spray liquid is condensed and collected by the condenser 7, stored in the
前述の被覆操作は流動中の粒状尿素の温度が60℃に達した時点から開始し、被覆量が最終の被覆肥料に対して12重量%となるまで行った。その後、粒子温度を60±2℃に維持することに留意して熱風の温度調節をしながら10分間熱風のみを吹き付けて乾燥を実施した。乾燥が終了した時点で被覆された粒状尿素を流動層1の最下部にある抜き出し口13より排出し、脱溶媒処理を経て溶出速度をコントロールする被覆層を有する被覆肥料(被覆尿素)を得た。
The above-mentioned coating operation was started from the time when the temperature of the flowing granular urea reached 60° C., and was carried out until the coating amount was 12% by weight based on the final coated fertilizer. Thereafter, while keeping in mind that the particle temperature was maintained at 60±2° C., only the hot air was blown for 10 minutes while controlling the temperature of the hot air to perform drying. When the drying was completed, the coated granular urea was discharged from the
被覆層の形成条件
粒状尿素:15kg
被覆中の粒子温度:60℃
溶解温度:100〜110℃
噴霧液温度:80〜100℃
熱風温度:130〜140℃
スプレー流速:108kg/h
2.被覆層表面の浮上防止処理
(実施例1)
予め粉砕機(商品名ミルサーIFM−800DG、岩谷産業社製)にて、塩化カリウムを30秒間粉砕、篩分して微粉末を得た。「1.被覆肥料の作製」で得られた被覆尿素100重量部を製造後速やかに回転ドラム式転動装置(直径90mm)に入れ、続いて25μm未満で篩い分けた塩化カリウム微粉末を0.3重量部添加した。60rpmで10分間転動し被覆尿素の表面に付着させることによって、本発明品の被覆粒状肥料(実施例1)を得た。なお、塩化カリウムの25℃の水に対する溶解度は36重量%である。
Conditions for forming coating layer Granular urea: 15 kg
Particle temperature during coating: 60°C
Melting temperature: 100-110°C
Spray liquid temperature: 80-100°C
Hot air temperature: 130-140°C
Spray flow rate: 108kg/h
2. Floating prevention treatment of coating layer surface (Example 1)
A pulverizer (trade name: Millser IFM-800DG, manufactured by Iwatani Sangyo Co., Ltd.) was used to pulverize potassium chloride for 30 seconds and sieve the powder to obtain a fine powder. 100 parts by weight of the coated urea obtained in “1. Preparation of coated fertilizer” was immediately put into a rotary drum type rolling device (diameter 90 mm) after the production, and then potassium chloride fine powder sieved to less than 25 μm was added. 3 parts by weight was added. A coated granular fertilizer of the present invention (Example 1) was obtained by rolling at 60 rpm for 10 minutes to adhere to the surface of the coated urea. The solubility of potassium chloride in water at 25°C is 36% by weight.
(実施例2)
「2.被覆層表面の浮上防止処理」において、25μm以上、150μm以下で篩い分けた塩化カリウム微粉末を用い、その添加量を0.1重量部に替える以外は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例2)を得た。
(Example 2)
In "2. Floating prevention treatment of coating layer surface", the treatment is carried out in the same manner as in Example 1 except that fine powder of potassium chloride sieved at 25 µm or more and 150 µm or less is used and the addition amount is changed to 0.1 part by weight. Thus, the coated granular fertilizer of the present invention (Example 2) was obtained.
(実施例3)
「2.被覆層表面の浮上防止処理」において、25μm以上、150μm以下で篩い分けた塩化カリウム微粉末を用い、その添加量を0.5重量部に替える以外は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例3)を得た。
(Example 3)
In "2. Floating prevention treatment of coating layer surface", the treatment is carried out in the same manner as in Example 1 except that potassium chloride fine powder sieved at 25 µm or more and 150 µm or less is used and the addition amount is changed to 0.5 part by weight. Thus, the coated granular fertilizer of the present invention (Example 3) was obtained.
(実施例4)
「2.被覆層表面の浮上防止処理」において、25μm以上、150μm以下で篩い分けた塩化カリウム微粉末を用い、その添加量を1.0重量部に替える以外は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例4)を得た。
(Example 4)
In "2. Floating prevention treatment of coating layer surface", the treatment is carried out in the same manner as in Example 1 except that potassium chloride fine powder sieved at 25 µm or more and 150 µm or less is used and the addition amount is changed to 1.0 part by weight. Thus, the coated granular fertilizer of the present invention (Example 4) was obtained.
(実施例5)
「2.被覆層表面の浮上防止処理」において、150μmより大で篩い分けた塩化カリウム微粉末を用い、その添加量を0.3重量部に替える以外は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例5)を得た。
(Example 5)
In “2. Floating prevention treatment of coating layer surface”, by treating according to Example 1 except that potassium chloride fine powder sieved with a size larger than 150 μm is used and the addition amount is changed to 0.3 part by weight. A coated granular fertilizer (Example 5) of the present invention was obtained.
(実施例6)
「2.被覆層表面の浮上防止処理」において、塩化カリウムを硫酸カリウムに替え、それ以外の条件は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例6)を得た。なお、硫酸カリウムの25℃の水に対する溶解度は12重量%である。
(Example 6)
In "2. Floating prevention treatment of coating layer surface", potassium chloride was replaced with potassium sulfate, and the other conditions were treated according to Example 1, to obtain the coated granular fertilizer of the present invention (Example 6). Obtained. The solubility of potassium sulfate in water at 25° C. is 12% by weight.
(実施例7)
「2.被覆層表面の浮上防止処理」において、25μm未満で篩い分けた塩化カリウム微粉末を、25μm以上、150μm以下で篩い分けた硫酸カリウム微粉末に替え、それ以外の条件は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例7)を得た。
(Example 7)
In “2. Floating prevention treatment of coating layer surface”, the potassium chloride fine powder sieved at less than 25 μm was replaced with potassium sulfate fine powder sieved at 25 μm or more and 150 μm or less, and other conditions were the same as in Example 1. A coated granular fertilizer of the present invention (Example 7) was obtained by processing according to the above method.
(実施例8)
「2.被覆層表面の浮上防止処理」において、25μm未満で篩い分けた塩化カリウム微粉末を、25μm以上、150μm以下で篩い分けた硫酸カリウム微粉末に替え、その添加量を0.05重量部に替え、それ以外の条件は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例8)を得た。
(Example 8)
In “2. Floating prevention treatment of coating layer surface”, the potassium chloride fine powder sieved at less than 25 μm is replaced with potassium sulfate fine powder sieved at 25 μm or more and 150 μm or less, and the addition amount is 0.05 part by weight. In place of the above, other conditions were treated according to Example 1 to obtain a coated granular fertilizer of the present invention (Example 8).
(実施例9)
「2.被覆層表面の浮上防止処理」において、25μm未満で篩い分けた塩化カリウム微粉末を、25μm以上、150μm以下で篩い分けた硫酸カリウム微粉末に替え、その添加量を1重量部に替え、さらにコーンスターチ(粒子径2〜30μm、平均粒径15μm)を0.1重量部混合して使用し、それ以外の条件は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例9)を得た。
(Example 9)
In “2. Floating prevention treatment of coating layer surface”, the potassium chloride fine powder sieved at less than 25 μm was replaced with the potassium sulfate fine powder sieved at 25 μm or more and 150 μm or less, and the addition amount was changed to 1 part by weight. Further, 0.1 part by weight of cornstarch (particle size 2 to 30 μm, average particle size 15 μm) was mixed and used, and the other conditions were treated according to Example 1 to obtain the coated granular fertilizer of the present invention. (Example 9) was obtained.
(実施例10)
「2.被覆層表面の浮上防止処理」において、25μm未満で篩い分けた塩化カリウム微粉末を、150μmより大で篩い分けた硫酸カリウム微粉末に替え、その添加量を0.3重量部に替え、それ以外の条件は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例10)を得た。
(Example 10)
In “2. Floating prevention treatment of coating layer surface”, the potassium chloride fine powder sieved at less than 25 μm was replaced with potassium sulfate fine powder sieved at more than 150 μm, and the addition amount was changed to 0.3 parts by weight. The other conditions were treated according to Example 1 to obtain a coated granular fertilizer of the present invention (Example 10).
(実施例11)
「2.被覆層表面の浮上防止処理」において、25μm未満で篩い分けた塩化カリウム微粉末を、25μm以上、150μm以下で篩い分けた炭酸ナトリウム微粉末に替え、それ以外の条件は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例11)を得た。なお、炭酸ナトリウムの25℃の水に対する溶解度は31重量%である。
(Example 11)
In “2. Floating prevention treatment of coating layer surface”, the potassium chloride fine powder sieved at less than 25 μm was replaced with sodium carbonate fine powder sieved at 25 μm or more and 150 μm or less, and other conditions were the same as in Example 1. The coated granular fertilizer of the present invention (Example 11) was obtained by processing according to the above method. The solubility of sodium carbonate in water at 25°C is 31% by weight.
(実施例12)
「2.被覆層表面の浮上防止処理」において、25μm未満で篩い分けた塩化カリウム微粉末を、25μm以上、150μm以下で篩い分けた塩化ナトリウム微粉末に替え、それ以外の条件は実施例1に準じて処理することによって、本発明品の被覆粒状肥料(実施例12)を得た。なお、塩化ナトリウムの25℃の水に対する溶解度は36重量%である。
(Example 12)
In “2. Floating prevention treatment of coating layer surface”, the potassium chloride fine powder sieved at less than 25 μm was replaced with sodium chloride fine powder sieved at 25 μm or more and 150 μm or less, and other conditions were the same as in Example 1. By treating according to the same manner, a coated granular fertilizer of the present invention (Example 12) was obtained. The solubility of sodium chloride in water at 25°C is 36% by weight.
(比較例1)
浮上防止処理を行っていない被覆肥料、すなわち「1.被覆肥料の作製」で得られた被覆尿素そのものを対照品の被覆粒状肥料(比較例1)とした。
(Comparative Example 1)
The coated fertilizer that was not subjected to the anti-floating treatment, that is, the coated urea itself obtained in “1. Preparation of coated fertilizer” was used as a coated granular fertilizer as a control product (Comparative Example 1).
(比較例2)
「2.被覆層表面の浮上防止処理」において、塩化カリウム(粒径25μm未満)をカオリン(関東化学社製、平均粒径1μm)に変更する以外は、実施例1に準じて対照品の被覆粒状肥料(比較例2)を得た。
(Comparative example 2)
In "2. Floating prevention treatment of coating layer surface", the coating of the control product was carried out according to Example 1 except that potassium chloride (particle diameter less than 25 µm) was changed to kaolin (Kanto Chemical Co., Inc., average particle diameter 1 µm). A granular fertilizer (Comparative Example 2) was obtained.
(比較例3)
「2.被覆層表面の浮上防止処理」において、塩化カリウム(粒径25μm未満)をシリカフューム(巴工業社製、平均粒径1μm)に変更する以外は、実施例1に準じて対照品の被覆粒状肥料(比較例3)を得た。
(Comparative example 3)
In “2. Floating prevention treatment of coating layer surface”, the coating of the control product was carried out in accordance with Example 1 except that potassium chloride (particle size less than 25 μm) was changed to silica fume (made by Tomoe Kogyo Co., Ltd., average particle size 1 μm) A granular fertilizer (Comparative Example 3) was obtained.
(比較例4)
「2.被覆層表面の浮上防止処理」において、塩化カリウム(粒径25μm未満)をベントナイト(関東化学社製、粒径50μm未満)に変更する以外は、実施例1に準じて対照品の被覆粒状肥料(比較例4)を得た。
(Comparative example 4)
In "2. Floating prevention treatment of coating layer surface", coating of the control product was carried out according to Example 1 except that potassium chloride (particle size less than 25 µm) was changed to bentonite (Kanto Chemical Co., Inc., particle size less than 50 µm). A granular fertilizer (Comparative Example 4) was obtained.
3.水溶性無機粉体の保持量の定量
上記実施例の各サンプルについて、下記方法により、水溶性無機粉体の保持量の定量を行なった。なお、定量結果から、「保持量」は上述した実施例の浮上防止処理における「添加量」とほぼ一致した。
3. Quantification of Retained Amount of Water-Soluble Inorganic Powder With respect to each sample of the above-mentioned examples, the retained amount of the water-soluble inorganic powder was quantified by the following method. From the quantitative results, the "retained amount" was almost the same as the "added amount" in the floating prevention treatment of the above-mentioned embodiment.
ビーカーにサンプル5gと純水100mlを入れ、10分間の超音波処理を行なった。処理後の水溶液について、イオンクロマトグラフィー(東ソー社製、IC2001)で水溶性無機粉体の濃度を測定した。一方、ブランクとして、水溶性無機粉体を用いた浮上防止処理を行っていない被覆肥料について同様の操作を行い、水溶性無機粉体の濃度を測定した。サンプルの測定濃度からブランクの測定濃度を差し引いた値から、サンプルが保持していた水溶性無機粉体の重量に換算し、被覆肥料100重量部に対する割合を求めた。 5 g of the sample and 100 ml of pure water were placed in a beaker and subjected to ultrasonic treatment for 10 minutes. With respect to the aqueous solution after the treatment, the concentration of the water-soluble inorganic powder was measured by ion chromatography (TO2001, IC2001). On the other hand, as a blank, the same operation was performed on the coated fertilizer using the water-soluble inorganic powder that was not subjected to the floating prevention treatment, and the concentration of the water-soluble inorganic powder was measured. The value obtained by subtracting the measured concentration of the blank from the measured concentration of the sample was converted into the weight of the water-soluble inorganic powder held by the sample, and the ratio to 100 parts by weight of the coated fertilizer was obtained.
4.評価方法
上記実施例および比較例の被覆粒状肥料について、製造後半年以上経過後のサンプルを用いて、下記評価を行なった。
4. Evaluation method The coated granular fertilizers of the above-mentioned Examples and Comparative Examples were evaluated as follows by using the samples obtained after the lapse of half a year or more after the production.
(a)固結率の測定
17.5cm×17.5cmのポリエチレン製の袋にサンプル500gを入れヒートシールした。40℃、30kgの重りで荷重をかけて2日間保存した。重りを静かに取り除き、サンプルに衝撃を与えないように静かに袋の外側を切った。ハケを使用して、サンプルの固結部分を取り出し、重量を測定して固結率(%)を求めた。固結率の値より固結評価を◎○×の3段階で判定した。固結評価が◎または○すなわち固結率が35%未満であれば合格とする。
(A) Measurement of solidification rate 500 g of a sample was put in a 17.5 cm×17.5 cm polyethylene bag and heat-sealed. The sample was stored under a load of 40 kg at a weight of 30 kg for 2 days. The weight was gently removed and the bag was gently cut to avoid impacting the sample. The solidified portion of the sample was taken out using a brush and the weight was measured to determine the solidification rate (%). Based on the value of the caking rate, the caking evaluation was judged in three grades of ◎○×. If the caking evaluation is ⊚ or ◯, that is, the caking rate is less than 35%, the test is passed.
固結率(%)=(固結部分の重量/全重量)×100
固結評価
固結率 0〜10% :◎
固結率 10〜35%:○
固結率 35%以上 :×
(b)発塵量の測定
蓋付きのポリプロピレン製容器(幅200mm、奥行き150mm、高さ210mm)の蓋の中央に上記サンプルを投入するための穴(直径40mm)を開け、空気抜き用の穴(直径15mm)をその横に開けた。そしてポリプロピレン製容器に蓋をして、蓋の中央の穴からロート(脚下径35mm)を用いてサンプル1kgを容器内に投入し、容器内の粉塵量を目視にて◎○×の3段階で判定した。発塵評価が◎または○であれば合格とする。
発塵評価
目視でほとんどなし〜タバコの煙程度:◎
目視で煙がもうもうとたつ程度:○
目視で煙がひどくもうもうとたつ程度:×
(c)浮上率の測定
風乾した2mmパスの黒ボク土100gにサンプル50粒を混合した後、16cm×20cmのバットに広げ、300mlの水を注いだ。バットを軽く振動させて、水面に浮上している粒数の割合を浮上率として求め、浮上性を◎○×の3段階で判定した。浮上評価が◎または○、すなわち浮上率が30%未満であれば合格とする。
浮上率(%)=(浮上粒数/全粒数)×100
浮上評価
浮上率 0〜20% :◎
浮上率 20〜30%:○
浮上率 30%以上 :×
(d)総合判定
固結、発塵、浮上の評価が全て◎であるものを◎、1つでも○があれば○、1つでも×があれば×と判定した。◎または○評価であれば合格とする。結果を表1に示す。判定の結果、水溶性無機粉体で被覆層の表面処理を行った被覆粒状肥料(実施例)はすべて、◎または○の判定であった。これに対して、水溶性無機粉体で被覆層の表面処理を行っていない被覆粒状肥料(比較例)はすべて×の判定であった。
Solidification rate (%) = (weight of solidified portion/total weight) x 100
Consolidation evaluation
Solidification rate 0 to 10%: ◎
Solidification rate 10-35%: ○
Solidification rate 35% or more: ×
(B) Measurement of Dust Generation A polypropylene container with a lid (width 200 mm, depth 150 mm, height 210 mm) has a hole (diameter 40 mm) for introducing the sample in the center of the lid, and a hole for venting air ( A diameter of 15 mm) was opened beside it. Then, the polypropylene container is covered, and 1 kg of the sample is put into the container from the hole in the center of the cover using a funnel (lower leg diameter 35 mm), and the amount of dust in the container is visually observed in three stages of ◎○×. It was judged. If the dust generation evaluation is ◎ or ○, it passes.
Dust generation evaluation Almost no visual observation ~ cigarette smoke level: ◎
Smoke is visually noticeable: ○
Smell is visually severe and sick: ×
(C) Measurement of levitation ratio After mixing 50 g of the sample with 100 g of black soil of 2 mm path that was air-dried, the sample was spread on a 16 cm x 20 cm vat and 300 ml of water was poured. The bat was vibrated lightly, and the ratio of the number of particles floating on the water surface was obtained as the levitation ratio, and the levitation property was evaluated in three grades of ⊚∘. If the floatation evaluation is ⊚ or ◯, that is, if the floatation rate is less than 30%, it is considered as pass.
Floating rate (%) = (number of floating particles/total number of particles) x 100
Levitation evaluation Levitation rate 0 to 20%: ◎
Ascent rate 20 to 30%: ○
Levitation rate 30% or more: ×
(D) Comprehensive Evaluation When all of the evaluations of consolidation, dust generation, and floatation were ⊚, ⊚ was evaluated as ◯ if there was at least one ◯, and as x if there was at least one x. Passed if ◎ or ○ evaluation. The results are shown in Table 1. As a result of the judgment, all the coated granular fertilizers (Examples) in which the coating layer was surface-treated with the water-soluble inorganic powder were judged as ⊚ or ○. On the other hand, all the coated granular fertilizers (comparative examples) in which the surface treatment of the coating layer was not performed with the water-soluble inorganic powder were evaluated as x.
この結果から、被覆層の表面に水溶性無機粉体を保持させることによって、長期保管後も施用時に粒状肥料の水面への浮上防止効果を有するとともに、固結防止効果と発塵防止効果も併せ持つ被覆粒状肥料が得られることが明らかである。また、水溶性無機粉体としては、様々なアルカリ金属またはアルカリ土類金属の無機酸塩またはハロゲン化物の組み合わせが利用できることが分かる。さらに、粒子径及び付着量を至適範囲に調整すれば、浮上防止効果、固結防止効果および発塵防止効果を高い水準(◎評価)で同時に満たすことができることも分かる。 From this result, by holding the water-soluble inorganic powder on the surface of the coating layer, it has an effect of preventing the granular fertilizer from floating on the water surface even after long-term storage, and also has an effect of preventing solidification and dust generation. It is clear that a coated granular fertilizer is obtained. Moreover, it is understood that various combinations of inorganic acid salts or halides of alkali metals or alkaline earth metals can be used as the water-soluble inorganic powder. Furthermore, it can be seen that if the particle size and the amount of adhesion are adjusted to the optimum range, the floating prevention effect, the caking prevention effect, and the dust generation prevention effect can be simultaneously satisfied at a high level (⊚ evaluation).
1.流動層
2.スプレーノズル
3.粒子
4.熱風
5.噴霧液
6.集塵機
7.コンデンサー
8.ブロワー
9.溶解槽
10.ポンプ
11.タンク
12.ヒーター
13.抜き出し口
1. Fluidized bed 2. Spray
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