JPS58124704A - Granular chemical for agricultural and disinfection use - Google Patents
Granular chemical for agricultural and disinfection useInfo
- Publication number
- JPS58124704A JPS58124704A JP529682A JP529682A JPS58124704A JP S58124704 A JPS58124704 A JP S58124704A JP 529682 A JP529682 A JP 529682A JP 529682 A JP529682 A JP 529682A JP S58124704 A JPS58124704 A JP S58124704A
- Authority
- JP
- Japan
- Prior art keywords
- granules
- parts
- oil
- binder
- granular
- 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.)
- Pending
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は貯蔵経時期間中でも物理、化学的変化を受けず
に長期間安定性が維持できる農業用防疫用粒状薬剤に関
するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a granular drug for agricultural epidemic prevention that can maintain stability for a long period of time without undergoing physical or chemical changes even during storage.
最近、農薬用防疫用薬剤の病害虫防除、雑草防除及び施
肥に適用する際の省力化と環境汚染防止等の観点から、
散布機具の改良、大型化が計られ、また、散布方式とし
ても、手撒き施用から散布機、航空機による空中散布ま
で行われて来ている。この場合、散布による生薬の粉状
化による微粉末の漂流すなわちドリフトを防止し、主薬
の施用面以外の環境を保全し、かつ、生育中の作物に対
する薬害を避けなければならない。Recently, from the viewpoint of saving labor and preventing environmental pollution when applying agricultural chemicals for pest control, weed control, and fertilization,
Spraying equipment has been improved and enlarged, and spraying methods have ranged from manual spreading to aerial spraying using sprayers and aircraft. In this case, it is necessary to prevent drifting of the fine powder due to the powdering of the herbal medicine by spraying, to preserve the environment other than the surface where the main medicine is applied, and to avoid chemical damage to the growing crops.
これらの目的に合致する剤型として、粒状に成型した粒
状薬剤が農業用防疫用薬剤に多く使用されている。この
粒状剤は他の剤型である粉剤、水和剤、乳剤等に比較し
て、散布後の有効成分の濃度が比較的高濃度に濃縮され
た状態で施用され、施用後の天候、特に水分の垂直及び
水平的な移動、又は植物自体の成長、栄養分吸収時の生
理生態的な機能に伴って生理活性点に移動し、その効果
発現の過程をとるので、その作用が比較的長期間にわた
り残効性の高い薬剤型である。As a dosage form that meets these objectives, granular medicines formed into granules are often used for agricultural epidemic prevention medicines. Compared to other dosage forms such as powders, wettable powders, emulsions, etc., this granular agent is applied with a relatively high concentration of active ingredients after dispersion, and is particularly sensitive to weather conditions after application. Water moves vertically and horizontally, or moves to physiologically active points along with physiological and ecological functions during growth and nutrient absorption of the plant itself, and takes the process of exerting its effects, so its effects last for a relatively long period of time. It is a drug type with long-lasting residual effects.
このように、粒剤は対象病害中、雑草、作物及び適用場
所、特に土壌水分との関係、農業用薬剤の有効成分の作
用機構、理化学的性質、製剤中の有効成分濃度が種々興
なるので造粒の方法は多様であるが、現在として次のよ
うな方法が行われている。第1はエーリフヒ社の造粒機
又はロッジ1社の造粒機などによる転勤式造粒法である
。これは有効成分の所定量を粉末の増量剤、結合剤、崩
壊補助剤とともに水又は水と結合剤との混合液と練合し
所望の粒子状に上記造粒機により造粒成型した後、必要
に応じ乾燥し粒状剤とする方法、第2は押出成型機によ
る方法であり、有効成分を、前記第1の方法におけると
同様の増量剤、補助剤とともに、一般に0〜20%の水
を加えて捏和し、直径0.5〜1.7n(32〜9メ・
ノシュ)の小孔を有する金属板に押圧して押出し、乾燥
して後、解砕機にかけ、篩分は等で整粒する方法である
。第3は被覆法である。これは有効成分を直接もしり番
マ予め微粉砕粉末にした状態のものを、整粒した鉱物性
ないし植物性粒状物の表面に液状結合剤を用いて被覆せ
しめて粒状剤とする方法である。これらの造粒法により
、一般には散粒時の地表単位面積当りの必要分布密度か
ら粒度分布は0.1〜2fi(150〜90メツシユ)
のものが実用化されてl、Nる。In this way, granules are used to treat various diseases, weeds, crops, and where they are applied, especially the relationship with soil moisture, the mechanism of action of the active ingredient of the agricultural chemical, the physicochemical properties, and the concentration of the active ingredient in the preparation. There are various granulation methods, but the following methods are currently used. The first method is a transfer granulation method using a granulator manufactured by Ehrlich or a granulator manufactured by Lodge 1. This involves kneading a predetermined amount of the active ingredient with a powder extender, binder, and disintegration aid with water or a mixed solution of water and a binder, and then granulating and molding the mixture into desired particles using the above-mentioned granulator. The second method is to use an extrusion molding machine, where the active ingredient is mixed with the same fillers and adjuvants as in the first method, and generally 0 to 20% water. In addition, knead to make a diameter of 0.5-1.7n (32-9m).
In this method, the material is extruded by pressing it against a metal plate with small holes, dried, and then passed through a crusher, and the particles are sieved to size. The third method is the coating method. This is a method in which the active ingredient is directly pulverized into a fine powder and then coated on the surface of sized mineral or vegetable granules with a liquid binder to form granules. . With these granulation methods, the particle size distribution is generally 0.1 to 2fi (150 to 90 mesh) based on the required distribution density per unit area of the ground surface during granulation.
Many of these have been put into practical use.
上記の粒状剤を製造する方法を見ると、第1の造粒法に
おいては、粒径が2顛以下程度の細粒を得ることを目的
とする場合では、粒剤の粒径が不一いになり、第2の押
出成型法では粒径は揃う力(製造収率が85〜95%と
なり歩溜りが悪い欠点がある。さらに、これらの方法に
おいては造粒後の水分が比較的除去しにくいため、強力
な通風ないしは熱乾燥を要し、有効成分が水により化学
変化を起し易い場合、乾燥時蒸散し易い性質をもつもの
では、このような造粒方法は適当でない。Looking at the method for manufacturing the above granules, in the first granulation method, when the purpose is to obtain fine particles with a particle size of about 2 or less, the particle size of the granules is uneven. In the second extrusion molding method, the particle size is uniform (manufacturing yield is 85 to 95%, resulting in poor yield).Furthermore, in these methods, water is relatively removed after granulation. This granulation method is not suitable if the active ingredient is easily chemically changed by water or tends to evaporate during drying.
また、第3の被覆法においては、現在上としてベントナ
イトや珪藻土のごとき多孔吸収性あるいは水中崩壊膨潤
性のある粒状物、或は珪石、火山礫、大理石等の比較的
吸水吸油性の少ないもの、或は天然土石粒にその目的に
あった水を初めとする灯油、機械油、動植物油等の天然
或は合成油又は油状の液体を結合剤として次工程で有効
成分を被覆させる等の方法で多様に製造されている。し
かもこの被覆法によって製造される粒剤はその経済的な
評価の面から解析すれば、(111i料が安価に大量に
均一な品質で得られること。(2)造粒時に低エネルギ
ーで得られること即ち造粒所要時間が短かく乾燥工程を
必要とせず目的とする粒度のものが高収率で得られるこ
と。(3)粒状薬剤が貯蔵期間中有効成分の分解を始め
被覆粉状物の剥離による粉化や固結等の物理化学的性質
の劣化のないこと。In addition, in the third coating method, granular materials such as bentonite and diatomaceous earth that have porous absorption properties or disintegrate and swell in water, or materials that have relatively low water and oil absorption properties such as silica stone, volcanic lapilli, and marble; Alternatively, the active ingredient can be coated in the next step by using natural or synthetic oils or oily liquids such as water, kerosene, machine oil, animal and vegetable oils, etc., as a binder, as well as water suitable for the purpose. Manufactured in a variety of ways. Moreover, if we analyze the granules produced by this coating method from the viewpoint of economic evaluation, (111i material can be obtained in large quantities at low cost and with uniform quality. (2) It can be obtained with low energy during granulation. In other words, the time required for granulation is short, and the desired particle size can be obtained at a high yield without the need for a drying process. (3) During storage, the active ingredient of the granular drug begins to decompose and the coated powder is dissolved. No deterioration of physicochemical properties such as powdering or caking due to peeling.
(4)散粒労力が少くその生理活性効果がもたらず経済
効果が最大のこと等があげられる。(4) It requires less labor to disperse particles, does not produce physiologically active effects, and has the greatest economic effect.
このように、被覆法による造粒は前2者に比し農業用防
疫用粒状薬剤として多くの長所を有するものであるが、
液状の結合剤がその薬剤の品質を左右するものであるた
め、基粒の種類性質等により、それぞれ結合剤を選択し
なければならない等の欠点もあった。As described above, granulation using the coating method has many advantages over the former two methods as a granular drug for agricultural epidemic prevention.
Since the liquid binder determines the quality of the drug, there are also drawbacks such as the need to select a binder depending on the type and nature of the base particles.
そこで、本発明者らは、どの基粒においても普遍的に用
いることのできる被覆用液状結合剤を得る目的で鋭意研
究の結果、結合剤として、液状鉱物油、可塑剤、半乾性
乃至不乾性の動植物油脂に界面活性剤を加えた不乾性乃
至半乾性液体を用いて被覆法により粒状農業用防疫用薬
剤を製造したところ、如何なる基粒にも適合する粒状薬
剤を製造することができることを見い出し本発明を完成
した。Therefore, as a result of intensive research with the aim of obtaining a coating liquid binder that can be universally used for any base grain, the present inventors have found that as a binder, liquid mineral oil, a plasticizer, semi-drying to non-drying When producing granular agricultural epidemic prevention chemicals using a coating method using a non-drying to semi-drying liquid made by adding surfactants to animal and vegetable oils and fats, it was discovered that granular chemicals compatible with any base grains could be produced. The invention has been completed.
本発明は、粒度0.1〜2.0額の無機、有機粒状物に
、液状の鉱物油、可塑剤および液状の半乾性乃至不乾性
の動植物油脂の1種または2種以上に界面活性剤を加え
た液状物を被覆し、その表面に粉末状農業用防疫用薬剤
の有効成分を粉衣した農業用防疫用粒状薬剤である。The present invention uses inorganic or organic granules with a particle size of 0.1 to 2.0, a liquid mineral oil, a plasticizer, and one or more liquid semi-drying to non-drying animal and vegetable oils and fats, and a surfactant. This is a granular agent for agricultural epidemic prevention, in which the active ingredient of the powdered agricultural epidemic prevention agent is coated on the surface of a liquid substance containing .
本発明に使用する粒基となる無機、有機粒状物は火成岩
、高成岩、水成岩、大理石岩等の砕石、陶磁、耐火物等
の窯業製品の砕粒、粒状尿素、無機塩粒状物、バガス粒
、米粒、タバコ屑粒、とうもろこし粒、大豆油かす等を
適宜の破砕機又は造粒機等によって粒度0.1〜2.0
鶴の粒径にそろえたものである。The inorganic and organic granular substances used as the granular base used in the present invention include crushed stones such as igneous rock, high volcanic rock, aqueous rock, and marble rock, crushed granules of ceramic products such as ceramics and refractories, granular urea, inorganic salt granules, bagasse grains, Rice grains, tobacco waste grains, corn grains, soybean oil cake, etc. are crushed to a particle size of 0.1 to 2.0 using an appropriate crusher or granulator.
It is made to match the grain size of Tsuru.
本発明に使用する被覆結合剤は鉱物油として灯油、マシ
ン油、スピンドル油、全冷油、発電製油、絶縁油、船舶
用機械油、流動パラフィン等、可塑剤として、ジブチル
フタレートのようなフタレート、トリフェニルフォスフ
ェートのようなフォスフェート等、半乾性乃至不乾性の
液状動植物油として、鯨油、ヒマシ油、オリーブ油、落
花生油、茶油、ナタネ油等があげられる。The coating binder used in the present invention includes mineral oils such as kerosene, machine oil, spindle oil, cold oil, power generation oil, insulating oil, marine machine oil, and liquid paraffin, and plasticizers such as phthalates such as dibutyl phthalate, Examples of semi-drying to non-drying liquid animal and vegetable oils, such as phosphates such as triphenyl phosphate, include whale oil, castor oil, olive oil, peanut oil, tea oil, and rapeseed oil.
以上の結合剤に添加する界面活性剤はポリオキンエチレ
ンノニルフjニルエーテルの如きポリオキシエチレンア
ルキルアリールエーテル、ソルビタン脂肪酸エステル、
ポリオキシエチレンソルビクン脂肪酸エステルの如き非
イオン界面活性剤、ドデシルベンゼンスルフオン酸カル
シウムの如きアニtン界m活性剤、)リメチルベンジル
アンモニウムクロライドの如きカチオン界面活性剤、セ
チルアミノアヤチックアシソド等の両性界面活性剤等を
単独又は適宜2種以上混合して用いることができる。そ
して、その添加量は大体結合剤に対し0.1%〜40%
程度であり、好適には0.5〜lO%である。The surfactants added to the above binder include polyoxyethylene alkylaryl ether such as polyoxyethylene nonyl phenyl ether, sorbitan fatty acid ester,
Nonionic surfactants such as polyoxyethylene sorbicun fatty acid esters, anionic surfactants such as calcium dodecylbenzenesulfonate, cationic surfactants such as lymethylbenzylammonium chloride, cetyl amino acid acid These amphoteric surfactants can be used alone or in an appropriate mixture of two or more. The amount added is approximately 0.1% to 40% of the binder.
It is preferably 0.5 to 10%.
本発明の粒状薬剤を製造するには、上記の粒度0.1〜
2.0額の無機、有機粒状物に、液状の鉱物油、可塑剤
又は液状の乾性乃至不乾性の動植物油脂に界面活性剤を
加えた液状物を粒状物に対し0.5〜40%程度、好適
には1〜15%混合し、粒状物の表面に十分被覆するよ
うにする。そして、別に農業用薬剤、防疫用薬剤の所定
量を略同量の担体例えばクレー、ホワイトカーボン、珪
藻土、ベントナイト、カオリン、タルク等の粉末と混和
するか、又は混合粉砕して、前記粒状物表面に被覆させ
て製造する。また、薬剤が粉体の場合は予め混合せずに
薬剤と担体を別々に粒状物表面に被覆してもよい。又界
面活性剤を含んだ油状物に有効、成分を常温又は加温し
て液状物にしたものを基粒に吸油後タルク等を粉衣して
製することも出来る。In order to produce the granular drug of the present invention, the above particle size is from 0.1 to
2.0 amount of inorganic or organic granules, liquid mineral oil, plasticizer, or liquid drying or non-drying animal or vegetable oil and fat with a surfactant added to the granules in an amount of about 0.5 to 40% , preferably 1 to 15%, so as to sufficiently coat the surface of the granules. Separately, a predetermined amount of an agricultural drug or an epidemic prevention drug is mixed with approximately the same amount of a carrier such as powder of clay, white carbon, diatomaceous earth, bentonite, kaolin, talc, etc., or mixed and pulverized, and the surface of the granules is Manufactured by coating. Furthermore, when the drug is a powder, the drug and carrier may be coated on the surface of the granules separately without being mixed in advance. It is also effective for oily substances containing surfactants, and can also be produced by making the ingredients into a liquid form at room temperature or heating them, absorbing the oil into base granules, and then coating with talc or the like.
本発明に用いる農業用、防疫用薬剤は液状、粉末状の公
知の薬剤は何れも用いることができる。As the agricultural and epidemic prevention chemicals used in the present invention, any known liquid or powdered chemicals can be used.
以上の如くして得られた本発明の農業用防疫用粒状薬剤
は製造直後ですでに安定な被覆層の接着強度が得られ、
貯蔵経時期間中でも、その物理化学特性は酸化等の化学
的な変化を全くうけず、長期間安定性を保持することが
できる。The agricultural epidemic prevention granular drug of the present invention obtained as described above already has a stable adhesive strength of the coating layer immediately after production,
Even during storage, its physicochemical properties do not undergo any chemical changes such as oxidation, and it can maintain stability for a long period of time.
次に本発明の実施例な示す。Next, examples of the present invention will be shown.
実施例1
粒度0.5〜1.7m(32〜10メソシユ)の砕石反
部に機械油2.91部、ポリオキシエチレンノニルフェ
ニルエーテル0.045部、ポリオキシエチレンドデシ
ルベンゼンエーテル0.03部及びドデシルベンゼンス
ルホン酸カルシウム0.015部のtll物を攪拌しな
がら、あらかじめオリゼメート (3−アリルオキシ−
1,2−ベンゾイソチアゾール−1,1−ジオキシド)
8B、クレー8部を混合粉砕した粉末16部を加えてオ
リゼメート8%粒剤を得る。Example 1 2.91 parts of machine oil, 0.045 parts of polyoxyethylene nonylphenyl ether, and 0.03 parts of polyoxyethylene dodecylbenzene ether were added to the surface of crushed stone with a particle size of 0.5 to 1.7 m (32 to 10 m). While stirring 0.015 parts of calcium dodecylbenzenesulfonate, oryzemate (3-allyloxy-
1,2-benziisothiazole-1,1-dioxide)
8B and 16 parts of a powder obtained by mixing and pulverizing 8 parts of clay were added to obtain 8% oryzemate granules.
実施例2
粒度0.5〜1.7m(32〜10メソシ5)の砕石8
9部に機械油2.9111、ポリオキシエチレンノニル
フェニルエーテル0.045部、ポリオキシエチレンド
デシルベンゼンエーテル0.03部、ドデシルベンゼン
スルホン酸カルシウムo 、o is部を攪拌しながら
加え、予めオリゼメート4部、クレー4部を混合粉砕し
た粉末8部を前記の処理を行った砕石粒に加え、被覆さ
せてオリゼメート4%粒剤を得る。Example 2 Crushed stone 8 with a particle size of 0.5 to 1.7 m (32 to 10 meso5)
To 9 parts, add 2.9111 parts of machine oil, 0.045 parts of polyoxyethylene nonylphenyl ether, 0.03 parts of polyoxyethylene dodecylbenzene ether, and 0 and 0 parts of calcium dodecylbenzenesulfonate with stirring. 8 parts of powder obtained by mixing and pulverizing 4 parts of clay and 4 parts of clay were added to the crushed stone grains subjected to the above treatment and coated to obtain 4% oryzemate granules.
実施例3
粒度0.5〜1.7寵(32〜10メ・ノシ:L)の海
砂90部にポリエチレンオキシ(E、0=5) ドデ
シルエーテル0.3部、スピンドル油1.7部を攪拌し
ながら加え、更にマーシェツト (2−クロロ−2′、
6′−ジエチル−N−ブトオキシメチルアセトアニリド
) 5部を加え、次にホワイトカーボン3部を粉衣して
マージエソ15%粒剤を得る。Example 3 90 parts of sea sand with a particle size of 0.5 to 1.7 cm (32 to 10 m/L), 0.3 part of polyethyleneoxy (E, 0=5) dodecyl ether, and 1.7 parts of spindle oil was added with stirring, and then Marchette (2-chloro-2',
Add 5 parts of 6'-diethyl-N-butoxymethylacetanilide and then coat with 3 parts of white carbon to obtain Marge Eso 15% granules.
実施例4
粒度0.5〜1.7fi(32〜10メツシユ)の海砂
89部にナタネ油2.5部、ポリオキシエチレン(E、
04モル)オクチルフェニルエーテル0.5部を攪拌し
ながら加えて海砂表面を湿潤させ、予めMIPC(2−
インプロビルフェニル−N−メチルカーバメート)4部
、クレー4部を混合粉砕した粉体な加えて粉衣してMI
PC4%粒剤を得る。Example 4 89 parts of sea sand with a particle size of 0.5 to 1.7 fi (32 to 10 mesh), 2.5 parts of rapeseed oil, polyoxyethylene (E,
0.5 part of octylphenyl ether (04 mol) was added with stirring to wet the sea sand surface,
Mix and crush 4 parts of Improbylphenyl-N-methylcarbamate) and 4 parts of clay, coat the powder, and mix.
Obtain PC4% granules.
実施例5
粒径0.5〜0.8鶴の天然珪石加、5部に予めピリダ
フェンチオン(ジエチルオキソフェニルピリダジンイル
キスホロチオエート) 10部、落花生油7部、ポリオ
キシエチレン(E、08モル)オクチルフェニルエーテ
ル0.5部のfi a 物ヲ約50℃に加温溶融液を添
加吸油させ、後0.046日以下のホワイトカーボン2
部を粉衣させ防疫用ピリダフェンチオン10%粒剤を得
る。Example 5 10 parts of pyridafention (diethyloxophenylpyridazine ilkis horothioate), 7 parts of peanut oil, and 08 mol of polyoxyethylene (E) were added to 5 parts of natural silica with a particle size of 0.5 to 0.8. ) A heated melt of 0.5 parts of octylphenyl ether at about 50°C was added to absorb the oil, and after 0.046 days or less white carbon 2
The mixture was coated with powder to obtain 10% pyridafention granules for epidemic prevention.
次に本発明の粒状剤が従来の粒状剤に比べその優位性を
示す実験並びに評価を記す。Next, experiments and evaluations showing the superiority of the granules of the present invention over conventional granules will be described.
被覆法による粒状薬剤の製法において、本発明の被覆結
合剤を用いて製造した粒剤(本発明品)、従来用いられ
ている被覆結合剤である、ポリビニルアルコール、カル
ボキシメチルセルローズ等の水溶解性高分子化合物の水
溶液を被覆結合剤として用いた粒剤(対照例1)、エチ
レングリコール、ポリプロピレングリコール等の水溶性
脂肪族多価アルコールを被覆結合剤として用いた粒剤(
対照例2)、灯油、機械油(ケロシン、潤滑油)を被覆
結合剤として用いた粒剤(対照例3)、天然動植物油特
に乾性油を被覆結合剤として用いた粒剤(対照例4)、
合成乾性油を被覆結合剤として用いた粒剤(対照例5)
、合成樹脂粘着溶液を被覆結合剤として用いた粒剤(対
照例6)の粒剤についての原料単価、製造エネルギー、
貯蔵安定性、生物効果についての評価を見れば下記第1
表の通りである。In the method of manufacturing granular drugs by coating method, granules produced using the coating binder of the present invention (product of the present invention), water-soluble coating binders such as polyvinyl alcohol, carboxymethyl cellulose, etc., which are conventionally used coating binders. Granules using an aqueous solution of a polymer compound as a coating binder (Control Example 1); Granules using a water-soluble aliphatic polyhydric alcohol such as ethylene glycol or polypropylene glycol as a coating binder (
Comparative Example 2), Granules using kerosene, machine oil (kerosene, lubricating oil) as a coating binder (Comparative Example 3), Granules using natural animal and vegetable oils, especially drying oils, as a coating binder (Comparative Example 4) ,
Granules using synthetic drying oil as coating binder (Control Example 5)
, raw material unit price, manufacturing energy, for granules using synthetic resin adhesive solution as coating binder (Control Example 6),
Looking at the evaluation of storage stability and biological effects, the following
As shown in the table.
第1表
各塊粒剤の経済的総合順位
註)各評価面より最良のものを1とした時の各順位数
ここに貯蔵安定性の項に粉化とあるのは、製造直後では
みられぬが、一定時間経過後結合剤が硬化等を始めとす
る変化の為、部分的に硬化、収縮等が起り粒剤被覆層と
基粒間との接着強度の弱化する部分が露呈されるという
結果、粉化と言う現象を呈するのである。これに対し本
発明品は長期間安定性を期待出来る不乾性即ち飽和化合
物よりなる被覆接合剤を使用しているので製造直後です
でに安定な被覆層の接着強度が得られ、貯蔵経時期間中
でもその物理化学特性は酸化等の化学的な変化を全くう
けず、長期間安定性を保持出来る。又対照例(2)のア
ルキレングリコール類を使用する方法は本発明の被覆結
合剤よりも上記圧が大きく、容器の開封時には消失して
粉化するおそれがある。Table 1 Economic overall ranking of each agglomerate (Note) Number of rankings when the best one from each evaluation aspect is taken as 1. Here, the term "powdery" in the storage stability section means that it is not observed immediately after manufacture. However, after a certain period of time, the binder undergoes changes such as hardening, resulting in partial hardening and shrinkage, exposing areas where the adhesive strength between the granule coating layer and the base grains is weakened. As a result, a phenomenon called powdering occurs. In contrast, the product of the present invention uses a non-drying coating bonding agent made of a saturated compound that can be expected to be stable for a long period of time, so the adhesive strength of the coating layer is already stable immediately after manufacturing, and even during storage. Its physicochemical properties are completely unaffected by chemical changes such as oxidation and can maintain stability for a long period of time. Furthermore, in the method using alkylene glycols in Comparative Example (2), the above-mentioned pressure is higher than that of the coated binder of the present invention, and there is a risk that the binder will disappear and turn into powder when the container is opened.
又対照例(3)は原料的には本発明品と同一素材を用い
るが、界面活性剤を含まず、その為に製造時のエネルギ
ー、特に造粒時間が長くかかり、又目的粒度域の粒剤製
品の度量も悪く施用後の生物硬化発現の時間がおそく全
体的な効果が劣る。又対照例(41,(51は原則的に
結合剤原料中に不飽和結合を有する不飽和化合物を含む
乾性油又は合成乾性油を結合剤とするので、前記貯蔵中
の酸化により、被覆層の効果が起り、この為粉化が起る
。Control example (3) uses the same material as the product of the present invention, but it does not contain a surfactant, so it takes a long time to produce, especially the granulation time, and the particles in the target particle size range. The dosage of the product is also poor, and the time to develop biocuring after application is slow, resulting in poor overall effectiveness. In addition, control examples (41, (51) basically use a drying oil containing an unsaturated compound having an unsaturated bond in the binder raw material or a synthetic drying oil as a binder, so the coating layer deteriorates due to oxidation during storage. effect occurs and hence powdering occurs.
又、製造工程中、風乾又は加熱乾燥工程を要し、又これ
により出来た粒状薬剤は水中又は土壌水分に溶解又は分
散されることがなく水不溶性の為に施用後の薬剤の均一
分散が妨げられ効果発現の時間も長時間を要する。又対
照例(6)は他に比し一般に高価なものが多く又毒性も
大きい、又その接着強度も硬化剤を使用したり、高温で
焼付をして硬化させるもので特別の工程を要し、その樹
脂の耐候性を慎重に選択しなければ、農業用の防疫用薬
剤の有効成分の効果発現に至らぬ無能な粒剤を製造する
危険性がある。今これらの被覆結合剤を前記グループ別
のものとして、下記のものを選んで粒状農薬オリゼメー
ト8粒剤を試作した。In addition, during the manufacturing process, an air drying or heat drying process is required, and the resulting granular drugs are not dissolved or dispersed in water or soil moisture, and their water insolubility prevents uniform dispersion of the drug after application. It also takes a long time for the effect to appear. Comparative example (6) is generally more expensive and more toxic than the others, and its adhesive strength requires a special process because it uses a hardening agent or is hardened by baking at high temperatures. Unless the weather resistance of the resin is carefully selected, there is a risk of producing incompetent granules that do not exhibit the effects of the active ingredients of agricultural epidemic prevention agents. Now, among these coating binders according to the above-mentioned groups, the following ones were selected to make eight granular pesticide Oryzemate granules.
被覆結合剤
本発明品
機械油、粘度詔、5センチボーズ 97部ポリオキシエ
チレン(E、04モル付加)ノニルフェニルエーテル
1.5部ポリオキシエチレン(E、On
=6) ドデシルエーテル
1.0部ドテシルベンゼンスルホン酸カルシウム
0.5部以上の混合液を本発明の被覆結合剤とした。Coating binder Inventive product Machine oil, viscosity, 5 cm Bose 97 parts polyoxyethylene (E, 04 mole addition) nonylphenyl ether
1.5 parts polyoxyethylene (E, On
=6) Dodecyl ether
1.0 parts Calcium dotesylbenzenesulfonate
0.5 part or more of the mixed liquid was used as the coating binder of the present invention.
本発明の対照品の被覆結合剤として下記のものを用いた
。The following was used as a coating binder for a control product of the present invention.
対照例1 ポリビニルアルコール(鹸化度88モル)5
%水溶液
対照例2 ポリピレングリコール
対照例3fi械油(粘度 路、5センチポーズ 50°
)対照例4 亜麻仁油
対照例5 ワニス
対照例6 尿素樹脂(65%固型分)
〔製法〕粒度0.5〜1.7關(32〜IOメソシユ)
の鉱物質砕石85部に上記被覆接合剤3部を平型攪拌機
に攪拌しながら加え全体を被覆接合剤でしめらしたのち
、予め、オリゼメート父%とクレー父%を混合粉砕した
製粉16部を粉衣被覆して製する。Control example 1 Polyvinyl alcohol (saponification degree 88 mol) 5
% aqueous solution control example 2 Polypyrene glycol control example 3fi machine oil (viscosity path, 5 centipause 50°
) Control example 4 Linseed oil control example 5 Varnish control example 6 Urea resin (65% solids) [Manufacturing method] Particle size 0.5-1.7 (32-IO mesh)
Add 3 parts of the above-mentioned coating binder to 85 parts of crushed mineral stone using a flat stirrer while stirring, and after soaking the whole with the coating binder, 16 parts of milled flour, which was prepared by mixing and pulverizing % oryzemate % and clay %, were mixed into powder. Manufactured by coating.
但し本発明品、対照品の磁2及び−3以外の磁1゜N1
4.m5及び陳6は1夜以上風乾して製した。However, magnetic 1°N1 other than magnetic 2 and -3 of the present invention product and control product
4. m5 and chen 6 were made by air drying for more than one night.
かくして製した稲熱病防除用オリヅメ−18%粒剤0.
5〜1.7m(32〜IOメソシユ)粒度を有する製品
の収率及び製品の水中脱離度、加温虐待保存後の有効成
分の分解率及び粉化率を次の方法によって測定した。The thus produced Orizume 18% granules for rice fever control 0.
The yield of a product having a particle size of 5 to 1.7 m (32 to IO m), the degree of desorption in water of the product, the decomposition rate and powdering rate of the active ingredient after storage under heating and abuse were measured by the following methods.
イ、水中脱離度
試料20gを精密に量り、標準硬水200mjを入れた
共栓付250m/のメスシリンダーに加える。B. Accurately weigh 20g of the underwater desorption sample and add it to a 250m graduated cylinder with a stopper containing 200mJ of standard hard water.
上下1回転を10秒の速さで5回転させた後、直ちに0
.15n+ (100メツシユ)のふるいを用いてふる
いつつ通過液を300mJ!のビーカー中に移す、磁器
攪拌器を用いて液をかき混ぜながら、その5部m7を正
確に300m1!の分液漏斗に移し、1(X)m#のエ
ーテルで抽出する。水層は更に第2.第3の各分液漏斗
に移し、エーテルで抽出する。水層番1捨てる。これら
のエーテル液を合わせ、無水硫酸ナトリウムを用いて脱
水後濾過する。容器及び濾紙上の残留物は少量のエーテ
ルで洗い洗液は濾液に合わせ、エーテルを留去する。残
留物にアセトンlQmjtを加えてとかし、1mj!を
薄層クロマトグラムグレートにスポットする。ベンゼン
:アセトン 7:3混液で展開する。保iIN比(Rf
)約0.64のオリゼメート層をかきとりアセトン25
mj!で抽出する。この液5 m Aに内部標準物質溶
液(ジイソブチルケトン0.3g/10m1!アセトン
)5mlを入れ、下記条件でガスクロマトグラフにかけ
オリゼメーF量(Amg)を算出し次式により水中脱離
度を算出する。Immediately after 5 rotations of 1 rotation up and down at a speed of 10 seconds,
.. Using a 15n+ (100 mesh) sieve, the liquid that passes through is sieved at 300 mJ! Using a porcelain stirrer, stir the liquid into a beaker of 5 m7 to exactly 300 m1! Transfer to a separatory funnel and extract with 1(X) m# of ether. The aqueous layer is further divided into the second layer. Transfer to a third separatory funnel and extract with ether. Discard water layer number 1. These ether solutions are combined, dehydrated using anhydrous sodium sulfate, and then filtered. The residue on the container and filter paper is washed with a small amount of ether, the washing liquid is combined with the filtrate, and the ether is distilled off. Add 1Qmjt of acetone to the residue and dissolve it to 1mj! Spot on the thin layer chromatogram grate. Develop with a 7:3 mixture of benzene:acetone. Protection iIN ratio (Rf
) Scrape off the oryzemate layer of about 0.64 and add acetone 25
mj! Extract with Add 5 ml of the internal standard substance solution (diisobutylketone 0.3 g/10 ml! acetone) to 5 mA of this solution, apply it to a gas chromatograph under the following conditions, calculate the amount of Oryzeme F (Amg), and calculate the degree of desorption in water using the following formula. .
オリゼメート Rt 5.2分
内部標準物質 Ht 2.2分
X200
水中脱離度%−X 100
試料20g中のオリゼメート量
(mg)
ガスクロマトグラフ操作条件
カラム担体;クロモソルプ W−AW DMC3液相
;5%シリコン OV −17
力ラム温度;21O。Oryzemate Rt 5.2 minutes Internal standard Ht 2.2 minutes x 200 Degree of desorption in water % - OV -17 Power ram temperature: 21O.
気化室;235゜
キャリヤガスi N2 、50m J /分検出器;水
素質イオン検出IF、1.D口、有効成分の残存率
製造当初のオリゼメート含量(g)に対する貯蔵経時後
の成分残存比(%)
但し、有効成分含量は試料5gをとり、アセトンlom
Jで抽出し、上澄液1ml1を前記薄層クロマトグラフ
に分は以下同様に操作して算出する。Vaporization chamber; 235° carrier gas i N2, 50 mJ/min Detector; hydrogen ion detection IF, 1. Port D, residual ratio of active ingredient The residual ratio of the ingredient after storage (%) to the oryzemate content (g) at the time of manufacture. However, the active ingredient content is determined by taking 5 g of a sample and
1 ml of the supernatant liquid was subjected to the thin layer chromatograph described above, and the amount was calculated in the same manner.
検量線は予めオリゼメート純品を用いて作成しておく。A calibration curve is prepared in advance using pure Oryzemate.
ハ、 粉化率
試料100gをとり、内径100mm、内fi100w
mのボールミル磁製ポットに入れ、これに総重置105
gの直径約30鶴の磁製ボール3個を入れ、毎分75回
転で15分間回転した後、0.3m(48メッシ:L)
のふるいを通過した量の比率を粉化率とする。C. Take 100g of powdering rate sample, inner diameter 100mm, inner fi 100w.
Place it in a ball mill porcelain pot of size 10m and place it on top of it for a total of 105cm.
Put 3 porcelain balls with a diameter of about 30 g and rotate at 75 revolutions per minute for 15 minutes, then 0.3 m (48 mesh: L)
The ratio of the amount passing through the sieve is the powdering rate.
これら特性値につき前記試作品の特性を検討して第2表
の結果を得た。The characteristics of the prototype were examined with respect to these characteristic values, and the results shown in Table 2 were obtained.
第 2 表
結合剤の差による粒剤特性値
以上の如く、本発明の粒状薬剤は他に比し格段のすぐれ
た特性値を有する。Table 2 Characteristic values of granules due to differences in binders As shown above, the granular drug of the present invention has much superior characteristic values compared to others.
次に本発明の粒剤が従来の被覆結合剤を用いて製造され
た粒剤に比し、有効成分の硬化の発揮がすぐれているこ
とを示す実験例をあげる。Next, an experimental example will be given showing that the granules of the present invention exhibit superior curing of the active ingredient compared to granules produced using conventional coating binders.
実験例1
供試粒剤
本発明品 実施例1のオリゼメート8%粒剤対照例1
実施例1の機械油、ポリオキシエチレンノニルフェニル
エーテル、ポリオキシエチレンドデシルベンゼンスルホ
ン酸カルシウム(以下、被覆結合剤と称す)の代りにカ
ルボオキシメチルセルローズ0.06部、水2.94部
(粘度700センチポーズ、鹸化値0.69)を用いた
他は実施例1と全く同様にして製造した粒剤
対照例2 実施例1の被覆結合剤の代りにポリグロビレ
ングリコール3部を用いた他は実施例1と全(同様にし
て製造した粒剤
対照例3 実施例1の被覆結合剤の代りにマシン油3部
を用いた他は実施例Iと全く同様にして製造した粒剤
対照例4 実施例1の被覆結合剤の代りにアマニ油3部
を用いた他は実施例1と全く同様にして製造した粒剤
対照例5 実施例1の被覆結合剤の代りにフェス(固体
骨75%)4部を用いた他は実施例1と全く同様にして
製造した粒剤
対照例6 実施例1の被覆結合剤の代りに尿素樹脂(固
体骨60%)5部を用いた他は実施例1と全く同様にし
て製造した粒剤
水稲品種:ニシホマレ
挿挾月日= 6月羽日
収穫月日:10月31日
耕種概要:栽植密度、15X3001m (22,2本
/if)施肥量:基油燐安280号(12−18−14
)10a当り、40 kg 、追肥8月14日、8月2
7日の2回同上肥料を10a当り20kg夫々施用した
。Experimental example 1 Test granules Present invention product Oryzemate 8% granules of Example 1 Control example 1
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity Granule control example 2, manufactured in exactly the same manner as in Example 1, except that 700 centipose and saponification value of 0.69) were used.3 parts of polyglobylene glycol was used in place of the coating binder of Example 1. Granule control example 3 manufactured in the same manner as in Example 1 Granule control example manufactured in the same manner as in Example I except that 3 parts of machine oil was used in place of the coating binder in Example 1 4 Granule control example 5 manufactured in exactly the same manner as in Example 1 except that 3 parts of linseed oil was used instead of the coating binder of Example 1. Granule control example 6 produced in exactly the same manner as in Example 1 except that 4 parts of urea resin (solid bone 60%) was used instead of the coating binder of Example 1. Granular paddy rice variety produced in exactly the same manner as Example 1: Nishihomare Cutting date = June Habi Harvesting date: October 31 Cultivation details: Planting density, 15 x 3001 m (22,2 plants/if) Fertilization amount: Base oil Phosphorus No. 280 (12-18-14
) per 10a, 40 kg, additional fertilizer August 14th, August 2nd
The same fertilizer was applied twice on the 7th at a dose of 20 kg per 10 a.
区劃面積:1区面積10rrl、各区波型畦畔板でかこ
った。Plot area: 1 plot area 10rrl, each plot surrounded by corrugated ridge boards.
散布月日及び散布量二8月13日に3kg/10aの量
を散粒した。Date of Spraying and Amount of Spraying: On August 13th, an amount of 3 kg/10a was sprinkled.
調査月日、方法:いもち病発病調査は9月詔日各区50
株につき、枝梗いもち罹病程度1/3以上及び1/3以
下の発痢穂率に分“けて調査した。白葉枯病発病調査は
9月3日各区25株につき上葉30葉につき発病葉牢及
びその病斑面積率を調査した。Survey date and method: Rice blast disease onset survey was conducted on September 5th day of the imperial edict in each ward.
Plants were investigated by dividing the incidence of panicles into those with branch rot disease severity of 1/3 or more and 1/3 or less.The investigation of the onset of white leaf blight was conducted on September 3rd, with the incidence of disease occurring on 30 upper leaves of 25 plants in each district. Leaf dungeons and their lesion area rates were investigated.
収量調査は10月31日収穫日に各区中心部3.3rr
r(73株)の精籾型(g)を調査した。The yield survey will be conducted on October 31st, the harvest day, at 3.3rr in the center of each district.
The spermatozoa type (g) of r (73 strains) was investigated.
調査成績を第3表で示す。The survey results are shown in Table 3.
実験例2
供試粒剤
本発明品 実施例2のオリゼメー14%粒剤対照例1
実施例2の機械油、ポリオキシエチレンノニルフェニル
エーテル、ポリオキシエチレンドデシルベンゼンスルホ
ン酸カルシウム(以下、被覆結合剤と称す)の代りにカ
ルボオキシメチルセルローズ0.06部、水2.94部
(粘度700センチボーズ、鹸化値0.69)を用いた
他は実施例2と全く同様にして製造した粒剤
対照例2 実施例2の被覆結合剤の代りにポリプロピレ
ングリコール3部を用いた他は実施例2と全く同様にし
て製造した粒剤
対照例3 実施例2の被覆結合剤の代りにマシン油3部
を用いた他は実施例2と全く同様にして製造した粒剤
対照例4 実施例2の被覆結合剤の代りにアマニ油3部
を用いた他は実施例2と全く同様にして製造した粒剤
対照例5 実施例2の被覆結合剤の代りにワニス(固体
分75%)4部を用いた他は実施例2と全く同様にして
製造した粒剤
対wA例6 実施例2の被覆結合剤の代りに尿素樹脂(
固体分間%)5部を用いた他は実施例2と全く同様にし
て製造した粒剤
以上の各粒剤を実験例1と同様の水稲品種、挿挾月日、
収穫月日、耕種概要、区制面積、散布月日、散布量及び
調査月日、方法により穂首いもち、枝梗いもちの発病状
況を調査した結果を第4表に示す。Experimental example 2 Test granules Present invention product Oryzeme 14% granules of Example 2 Control example 1
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity Granule control example 2, manufactured in exactly the same manner as in Example 2, except that 700 centiBose and saponification value of 0.69) were used.Execution example except that 3 parts of polypropylene glycol was used in place of the coating binder of Example 2. Granule control example 3 produced in exactly the same manner as in example 2 Granule control example 4 produced in exactly the same manner as in example 2 except that 3 parts of machine oil was used instead of the coating binder in example 2 Granule control example 5 produced in exactly the same manner as in Example 2 except that 3 parts of linseed oil was used in place of the coating binder in Example 2. Varnish (solid content 75%) 4 in place of the coating binder in Example 2 Example 6 Granules prepared in exactly the same manner as in Example 2 except that part of the urea resin was used instead of the coating binder of Example 2
The granules manufactured in exactly the same manner as in Example 2 except that 5 parts (solids content %) were used were mixed with the same paddy rice variety, inserting date, and the same as in Experimental Example 1.
Table 4 shows the results of investigating the disease onset status of panicle neck blast and branch blast blast based on harvest date, cultivation details, zoning area, application date, application amount, survey date, and method.
第4表
以上の実験例1.2により明らかなように、本発明の粒
剤は従来の被覆結合剤を用いた粒剤に比し、オリゼメー
ト8%及び4%の農薬剤の効果がすぐれている。As is clear from Experimental Example 1.2 in Table 4 and above, the granules of the present invention have superior effects on pesticides containing 8% oryzemate and 4% compared to granules using conventional coated binders. There is.
実験例3
供試粒剤
本発明品 実施例3のマージユツト5%粒剤対照品
カオリン79.5部、ベントナイト加部、ドデシルベン
ゼンスルホン酸ソータ0.511の混合粉体に水20部
を加えて捏造し押出造粒機にかけ、乾燥後0.5〜1.
7日(32〜10メツシユ)に篩分けて基粒を作る。こ
れより95部をとり、攪拌しなからマーシェツト5部を
吸油したマージユツト5%粒剤。Experimental Example 3 Test granules Present invention product Merge 5% granules control product of Example 3
Add 20 parts of water to a mixed powder of 79.5 parts of kaolin, part of bentonite, and 0.511 parts of dodecylbenzenesulfonic acid sorter, make the mixture, apply it to an extrusion granulator, and after drying, the powder will be 0.5 to 1.
On the 7th day (32 to 10 meshes), it is sieved to form base grains. From this, 95 parts were taken and, without stirring, 5 parts of marchet was absorbed to obtain a 5% granule.
水稲品種:健苗移植栽培ニシホマレ
播種月日: 5月28日、挿挾月日:′6月20日耕種
概要:栽植密度15 X 30cm (22,2本/r
rf)施肥量 基油硫安280号(12−18−4)1
0aあたり40kg施肥
区劃面積:1区10ホ各区波型畦畔板でかこった。Paddy rice variety: Healthy seedling transplant cultivation Nishihomare Sowing date: May 28th, Cutting date: 'June 20th Cultivation details: Planting density 15 x 30cm (22.2 plants/r)
rf) Fertilization amount Base oil ammonium sulfate No. 280 (12-18-4) 1
Fertilize 40kg per 0a Field area: 1 plot, 10 plots Each plot is surrounded by corrugated ridge boards.
施用月日及び量、方法:挿挾前3日、挿挾直後及び3日
後の3時期に各々3kg/10aの割合で土壌処理を行
った。Application date, amount, and method: Soil was treated at a rate of 3 kg/10 a at three times: 3 days before cutting, immediately after cutting, and 3 days after cutting.
調査時期、方法ニア月20日挿挾30日後の各区雑草種
別に、雑草を抜き取り、水洗、風乾後の生体量(g)を
秤量した。Survey period and method Weeds were cut out on the 20th of each month, and 30 days later, weeds were pulled out for each weed type, washed with water, and the biomass (g) after being air-dried was weighed.
調査結果を第5表に示す。The survey results are shown in Table 5.
第 5 表
以上の如く、本発明品は対照品よりも水田の一年生雑草
及び多年生雑草その他主要雑草の防除に効果があり、施
用時期も挿挾前3日〜当日迄の方が、挿挟3日後より効
果があった。Table 5 As shown above, the product of the present invention is more effective than the control product in controlling annual weeds, perennial weeds, and other major weeds in paddy fields, and it is more effective to control annual weeds, perennial weeds, and other major weeds in paddy fields than the control product. It was more effective after a day.
実験例4
供試粒剤
本発明品、実施例4のMIPC4%粒剤対照品 汚砂8
7部に石炭酸樹脂系接剤(固形分60%)5部を攪拌し
ながら加え、予めMIPC4部、クレー4部を混合粉砕
した粉体を加えて粉衣させ、65°±3℃で約2時間通
風乾燥させて得た粒剤
水稲品種:アソミノリ
挿挾月日: 6月20日
耕種概要:栽植密度15 X 30 cm基肥量塩基油
安280号(12−18−14) 10 a当り40
k+r施肥、8月り6日塩加燐安280号108当り2
0 kg施肥区制面積=1区20Onf各区波型畦畔板
でかこつtこ。Experimental Example 4 Test granules Invention product, MIPC 4% granule control product of Example 4 Dirty sand 8
Add 5 parts of carbolic acid resin adhesive (solid content 60%) to 7 parts with stirring, add powder prepared by mixing and pulverizing 4 parts of MIPC and 4 parts of clay in advance, coat with powder, and heat at 65°±3°C for about 2 hours. Granules obtained by air drying for hours Paddy rice variety: Asominori Date of insertion: June 20th Cultivation details: Planting density: 15 x 30 cm Base fertilizer amount: Base oil No. 280 (12-18-14) 40 per 10 a
k+r fertilization, August 6th Shioka Rin-an No. 280 No. 108 2
0 kg fertilization zone area = 1 zone 20 onf each zone with corrugated ridge board.
施用日時、量、方法: 8月1日、108当り3 kg
の調査時期及び方法27月31日(散布直前)8月2日
(散布1日後)8月15日(散布15日後)及び8月3
0日(散布□□□日後)に次の掬い取り法及び払い落し
法により防虫効果を調査した。Application date, amount, method: August 1st, 3 kg per 108
Survey timing and method2 July 31st (just before spraying) August 2nd (1 day after spraying) August 15th (15 days after spraying) and August 3rd
On day 0 (□□□ days after spraying), the insect repellent effect was investigated using the following scooping method and brushing off method.
掬い取り法:各区2プロットとして、口径361の捕虫
網を用いて各プロットより片振りで10回I20回掬い
取り、各区の害虫種別に計数した。Scooping method: Two plots were set in each plot, and using an insect net with a diameter of 361 mm, scoops were scooped out from each plot 10 times and 20 times in each plot, and the pests were counted according to the pest type in each plot.
払い落し法:各区3プロットとして各プロットから任意
に20株計60株を抽出し、粘着物を塗布しり18X2
5cm (85版大)の黒色セルロイド板に払い落し害
虫種類別に計数した。Wipe-off method: Arbitrarily extract 20 plants and a total of 60 plants from each plot as 3 plots in each area, and apply adhesive to them in a 18x2
The pests were brushed off onto a 5 cm (85 size) black celluloid board and counted by type.
掬い取り調査の結果を次の第6表に、払い落し調査の結
果を第7表に示す。The results of the scooping survey are shown in Table 6 below, and the results of the scraping survey are shown in Table 7.
第 6 表
第 7 表
以上の第6.第7表により明らかなように本発明品はヨ
コバイ、ウンカ類の防除に長期間にわたって効果があっ
た。Table 6, Table 7 and above, Section 6. As is clear from Table 7, the product of the present invention was effective in controlling leafhoppers and planthoppers over a long period of time.
実験例5
供試粒剤 実施例5の10%ピリダコエンチオン粒剤
対照例 実施例5の組成のポリオキシエチレン(E、0
8モル)オクチルフェニルエーテル0.5部の代りに落
花生油 合計使用量7.5部を同様に操作して製造した
粒剤
以上の各粒剤をキンバエ最終令幼虫20匹 水10m1
を入れた直径9cm高さ5■の腰高シャーレに各々1g
を入れ一定時間後の殺姐力をみた結果を第8表に示す。Experimental Example 5 Test Granules 10% Pyridacoenethione Granules Control Example of Example 5 Polyoxyethylene (E, 0
8 mol) Peanut oil in place of 0.5 part of octyl phenyl ether (Total usage: 7.5 parts) Each granule larger than the granules produced in the same manner was added to 20 last instar fly larvae and 10 ml of water.
1 g each in a waist-high petri dish with a diameter of 9 cm and a height of 5 cm.
Table 8 shows the killing power after a certain period of time.
第8表
以上の結果より本発明粒剤は対照粒剤より殺岨力が速効
的にあられれる。From the results shown in Table 8 and above, the granules of the present invention exhibit more rapid killing power than the control granules.
特許出願人 三笠化学工業株式会社
代理人 伊東寸志(ほか2名)
手続補正書
1、11牛のJしR
蒙57年特許願 第5296号
2、発明の名称
農業用防疫用粒状薬剤
3、 i正をする者
事件との関係 特許出願人
住所
4、代理人
明 細 書
1、発明の名称 農業用防疫用粒状薬剤2、特許請求の
範囲
■4粒度0.1〜2.0−の無機、有機粒状物に、液状
の鉱物油、可塑剤又は液状の半乾性乃至不乾性の動植物
油脂に界面活性剤を加えた液1尺物を被覆し、その表面
に粉末状農業用防疫用薬卯1を粉衣してなることを特徴
とする農業用防疫用粒状薬剤3、発明の詳細な説明
本発明は貯蔵経時期間中でも物理、化学豹変イヒを受け
ずに長期間安定性が維持できる農業用防疫用粒状薬剤に
関するものである。Patent Applicant Mikasa Chemical Industry Co., Ltd. Agent Sunshi Ito (and 2 others) Procedural Amendment 1, 11 Cow Jushi R Patent Application No. 5296 of Mongolia 1957 2, Title of Invention Granular Agent for Agricultural Epidemic Prevention 3, i Relationship with the person making the case: Address of the patent applicant: 4, Attorney's statement: 1, Title of the invention: Granular agent for agricultural epidemic prevention 2, Claims: ■4: Inorganic particles with a particle size of 0.1 to 2.0; The organic granules are coated with liquid mineral oil, plasticizer, or liquid semi-drying to non-drying animal and vegetable oil with a surfactant added, and the surface is coated with powdered agricultural epidemic prevention medicine 1. Detailed Description of the Invention The present invention provides a granular agent for agricultural epidemic prevention which is characterized by being coated with a powder and which maintains stability for a long period of time without undergoing sudden physical or chemical changes even during storage. The invention relates to granular drugs for use.
最近、農薬用防疫用薬剤の病害虫防除、雑草防除及び施
肥に通用する際の省力化と環境ン引染防止等の観点から
、散布機具の改良、大型化力1十られ、また、散布方式
としても、手撒き施用から散布機、航空機による空中散
布まで行われて来てし)る。この場合、散布による主薬
の粉状化による微粉末の漂流すなわちドリフl、を防止
し、生薬の施用曲以外の環境を保全し、かつ、生育中の
作物にり4する薬害を避けなければならない。Recently, from the viewpoint of labor saving and prevention of environmental contamination when pest control agents for agricultural chemicals are used for pest control, weed control, and fertilization, spraying equipment has been improved and increased in size. Applications range from hand-spreading to aerial spraying using spray machines and aircraft. In this case, it is necessary to prevent drifting of fine powder due to the powdering of the main drug by spraying, preserve the environment other than the area where the herbal medicine is applied, and avoid chemical damage to growing crops. .
これらの目的に合致する剤型として、粒状に成型した粒
状薬剤が農薬用防疫用薬剤に多く使用されている。この
粒状剤は他の剤型である粉剤、水和剤、乳剤等に比較し
て、散布後の有効成分の濃度が比較的高濃度に濃縮され
た状態で施用され、施用後の天候、特に水分の垂直及び
水平的な移動、又は植物自体の成長、栄養分吸収時の生
理生態的な機能に伴って生理活性点に移動し、その効果
発現の過程をとるので、その作用が比較的長期間にわた
り残効性の高い薬剤型である。As a dosage form that meets these objectives, granular medicines formed into granules are often used as agricultural chemicals for epidemic prevention. Compared to other dosage forms such as powders, wettable powders, emulsions, etc., this granular agent is applied with a relatively high concentration of active ingredients after dispersion, and is particularly sensitive to weather conditions after application. Water moves vertically and horizontally, or moves to physiologically active points along with physiological and ecological functions during growth and nutrient absorption of the plant itself, and takes the process of exerting its effects, so its effects last for a relatively long period of time. It is a drug type with long-lasting residual effects.
このように、粒剤は対象病害中、雑草、作物及び通用場
所、特に土壌水分との関係、農業用薬剤 ”の有効成分
の作用機構、理化学的性質、製剤中の有効成分濃度が種
々異なるので造粒の方法は多様であるが、現在として次
のような方法が行われている。第1はエーリ・/ヒ社の
造粒機又はロノシエ社の造粒機などによる転勤式造粒法
である。これは有効成分の所定量を粉末の増量剤、結合
剤、崩壊補助剤とともに水又は水と結合剤との混合液と
練合し所望の粒子状に上記造粒機にまり造粒成型した後
、必要に応じ乾燥し粒状剤とする方法、第2は押出成型
機による方法であり、有効成分を、前記第1の方法にお
けると同様の増量剤、補助剤とともに、一般に0〜20
%の水を加えて捏和し、直径0.5〜1.7m(32〜
9メツシユ)の小孔を有する金属板に押圧して押出し、
乾燥して後、解砕機にかけ、篩分は等で整粒する方法で
ある。第3は被覆法である。これは有効成分を直接もし
くは予め微粉砕粉末にした状態のものを、整粒した鉱物
性ないし植物性粒状物の表面に液状結合剤を用いて被覆
せしめて粒状剤とする方法である。これらの造粒法によ
り、一般には散粒時の地表単位面積当りの必要分布密度
から粒度分布は0.1〜2fi(150〜90メソシユ
)のものが実用化されている。In this way, granules differ in their relationship with target diseases, weeds, crops, and where they are used, especially soil moisture, the mechanism of action of the active ingredients of agricultural chemicals, their physicochemical properties, and the concentration of active ingredients in the formulation. There are various methods of granulation, but the following methods are currently in use.The first is a transfer-type granulation method using a granulator manufactured by Eri/Hi or a granulator manufactured by Ronosier. This involves kneading a predetermined amount of the active ingredient with a powder extender, binder, and disintegration aid with water or a mixture of water and a binder, and then forming the desired particles into the above-mentioned granulator. The second method is to use an extrusion molding machine, and the active ingredient is mixed with the same fillers and adjuvants as in the first method, generally in a concentration of 0 to 20%.
% of water and knead to form a diameter of 0.5~1.7m (32~
9 meshes) and extruded by pressing on a metal plate having small holes.
After drying, it is passed through a crusher and sieved to size the particles. The third method is the coating method. This is a method in which the active ingredient is coated directly or in a pre-pulverized powder state onto the surface of sized mineral or vegetable granules using a liquid binder to form granules. These granulation methods have generally put into practical use a particle size distribution of 0.1 to 2 fi (150 to 90 mesos) based on the required distribution density per unit area of the earth's surface during granulation.
上記の粒状剤を製造する方法を見ると、第1の造粒法に
おいては、粒径が2龍以下程度の細粒を得ることを目的
とする場合では、粒剤の粒径が不揃いになり、第2の押
出成型法では粒径は揃うが製造収率が85〜95%とな
り歩溜りが悪い欠点がある。さらに、これらの方法にお
いては造粒後の水分が比較的除去しにくいため、強力な
通風ないしは熱乾燥を要し、有効成分が水により化学変
化を起し易い場合、乾燥時蒸散し易い性質をもつもので
は、このような造粒方法は適当でない。Looking at the method for producing the above granules, in the first granulation method, when the purpose is to obtain fine particles with a particle size of about 2 dragons or less, the particle size of the granules becomes irregular. In the second extrusion molding method, the particle size is uniform, but the manufacturing yield is 85 to 95%, which has the disadvantage of poor yield. Furthermore, in these methods, it is relatively difficult to remove water after granulation, so strong ventilation or heat drying is required, and if the active ingredient is easily chemically changed by water, it may have a tendency to evaporate during drying. Such a granulation method is not suitable for grains.
また、第3の被覆法においては、現在上としてベントナ
イトや珪藻土のごとき多孔吸収性あるいは水中崩壊膨潤
性のある粒状物、或は珪石、火山礫、大理石等の比較的
吸水吸油性の少ないもの、或は天然主石粒にその目的に
あった水を初めとする灯油、機械油、動植物油等の天然
或は合成油又は油状の液体を結合剤として次工程で有効
成分を被覆させる等の方法で多様に製造されている。し
かもこの被覆法によって製造される粒剤はその経済的な
評価の面から解析すれば、(11原料が安価に大量に均
一な品質で得られること。(2)造粒時に低エネルギー
で得られること即ち造粒所要時間が短かく乾燥工程を必
要とせず目的とする粒度のものが高収率で得られること
。(3)粒状薬剤が貯蔵期間中有効成分の分解を始め被
覆粉状物の剥離による粉化や固結等の物理化学的性質の
劣化のないこと。In addition, in the third coating method, granular materials such as bentonite and diatomaceous earth that have porous absorption properties or disintegrate and swell in water, or materials that have relatively low water and oil absorption properties such as silica stone, volcanic lapilli, and marble; Alternatively, the natural main stone grains are coated with the active ingredient in the next step by using water, natural or synthetic oils such as kerosene, machine oil, animal and vegetable oils, or oily liquids as a binder, depending on the purpose. are manufactured in a variety of ways. Furthermore, if we analyze the granules produced by this coating method from the viewpoint of economic evaluation, (11) the raw materials can be obtained in large quantities at low cost and with uniform quality; (2) the granules can be obtained with low energy during granulation; In other words, the time required for granulation is short, and the desired particle size can be obtained at a high yield without the need for a drying process. (3) During storage, the active ingredient of the granular drug begins to decompose and the coated powder is dissolved. No deterioration of physicochemical properties such as powdering or caking due to peeling.
(4)数粒労力が少くその生理活性効果がもたらす経済
効果が最大のこと等があげられる。(4) Few grains require less labor, and their physiologically active effects have the greatest economic effect.
このように、被覆法による造粒は前2者に比し農業用防
疫用粒状薬剤として多くの長所を有するものであるが、
液状の結合剤がその薬剤の品質を左右するものであるた
め、基粒の種類性質等により、それぞれ結合剤を選択し
なければならない等の欠点もあった。As described above, granulation using the coating method has many advantages over the former two methods as a granular drug for agricultural epidemic prevention.
Since the liquid binder determines the quality of the drug, there are also drawbacks such as the need to select a binder depending on the type and nature of the base particles.
そこで、本発明者らは、との基粒においても普遍的に用
いることのできる被覆用液状結合剤を得る目的で鋭意研
究の結果、結合剤として、液状鉱物油、可塑剤、半乾性
乃至不乾性の動植物油脂に界面活性剤を加えた不乾性乃
至半乾性液体を用いて被覆法により粒状農業用防疫用薬
剤を製造したところ、如何なる基粒にも適合する粒状薬
剤を製造することができることを見い出し本発明を完成
した。Therefore, as a result of intensive research with the aim of obtaining a liquid binder for coating that can be universally used in base grains of When a granular agricultural epidemic prevention agent was manufactured by a coating method using a non-drying to semi-drying liquid made by adding a surfactant to dry animal and vegetable oil, it was found that a granular agent compatible with any base grain could be manufactured. Heading Completing the Invention.
本発明は、粒度0.1〜2.0鶴の無機、有機粒状物に
、液状の鉱物油、可塑剤および液状の半乾性乃至不乾性
の動植物油脂の1種または2m以上に界面活性剤を加え
た液状物を被覆し、その表面に粉末状農業用防疫用薬剤
の有効成分を粉衣した農業用防疫用粒状薬剤である。In the present invention, one kind of liquid mineral oil, a plasticizer, and a liquid semi-drying to non-drying animal or vegetable oil or fat, or a surfactant is added to inorganic or organic granules having a particle size of 0.1 to 2.0 m. This is a granular agricultural epidemic prevention agent in which the added liquid is coated and the active ingredient of the powdered agricultural epidemic prevention agent is coated on the surface.
本発明に使用する粒基となる無機、有機粒状物は火成岩
、深成岩、水成岩、大理石岩等の砕石、陶磁、耐火物等
の窯業製品の砕粒、粒状尿素、無機塩粒状物、バガス粒
、米粒、タバコ屑粒、とうもろこし粒、大豆油かす等を
適宜の破砕機又は造粒機等によって粒度0.1〜2.0
寵の粒径にそろえたものである。The inorganic and organic granular substances used as the granular base used in the present invention include crushed stones such as igneous rock, plutonic rock, aqueous rock, and marble rock, crushed granules of ceramic products such as ceramics and refractories, granular urea, inorganic salt granules, bagasse grains, and rice grains. , tobacco waste grains, corn grains, soybean oil cake, etc., are crushed to a particle size of 0.1 to 2.0 using an appropriate crusher or granulator.
The particle size is adjusted to the desired size.
本発明に使用する被覆結合剤は鉱物油として灯油、マシ
ン油、スピンドル油、冷凍機油、タービン油、絶縁油、
船舶用機械油、流動パラフィン等、可塑剤として、ジブ
チルフタレートのようなフタレート、トリフェニルフォ
スフニー]・のようなフォスフェート等、半乾性乃至不
乾性の液状動植物油として、鯨油、ヒマシ油、オリーブ
油、落花生油、茶油、ナタネ油等があげられる。The coating binder used in the present invention includes mineral oils such as kerosene, machine oil, spindle oil, refrigeration oil, turbine oil, insulating oil,
Marine machine oil, liquid paraffin, plasticizers such as phthalates such as dibutyl phthalate, phosphates such as triphenylphosphny, semi-drying to non-drying liquid animal and vegetable oils such as whale oil, castor oil, olive oil. , peanut oil, tea oil, rapeseed oil, etc.
以上の結合剤に添加する界面活性剤はポリオキシエチレ
ンノニルフェニルエーテルの如きポリオキシエチレンア
ルキルアリールエーテル、ソルビタン脂肪酸エステル、
ポリオキシエチレンソルビタン脂肪酸エステルの如き非
イオン界面活性剤、ドデシルベンゼンスルフオン酸カル
シウムの如きアニオン界面活性剤、トリメチルベンジフ
レアンモニウムクロライドの如きカチオン界面活性剤、
セチルアミノアセチックアシ・ノド等の両性界面活性剤
等を単独又は適宜2種以上混合して用いることができる
。そして、その添加量は大体結合側番こ対し0.1%〜
40%程度であり、好適には0.5〜lO%である。The surfactants added to the above binder include polyoxyethylene alkylaryl ether such as polyoxyethylene nonylphenyl ether, sorbitan fatty acid ester,
Nonionic surfactants such as polyoxyethylene sorbitan fatty acid ester, anionic surfactants such as calcium dodecylbenzenesulfonate, cationic surfactants such as trimethylbenzifurammonium chloride,
Amphoteric surfactants such as cetyl aminoacetic acid can be used alone or in combination of two or more. The amount added is approximately 0.1% to the bond side number.
It is about 40%, preferably 0.5 to 10%.
本発明の粒状薬剤を製造するには、上記の粒度0.1〜
2.0fiの無機、有機粒状物に、液状の鉱物油、可塑
剤又は液状の乾性乃至不乾性の動植物油脂に界面活性剤
を加えた液状物を粒状物に対し0.5〜40%程度、好
適には1〜15%混合し、粒状物の表面に十分被覆する
ようにする。そして、別に農業用薬剤、防疫用薬剤の所
定量を略同量の担体例えばクレー、ホワイトカーボン、
硅凍土、ベントナイト、カオリン、タルク等の粉末と混
和するか、又は混合粉砕して、前記粒状物表面に被覆さ
せて製造する。また、薬剤が粉体の場合は予め混合せず
に薬剤と担体を別々に粒状物表面に被覆してもよい。又
界面活性剤を含んだ油状物に有効成分を常温又は加温し
て液状物にしたものを基粒に吸油後タルク等を粉衣して
製することも出来る。In order to produce the granular drug of the present invention, the above particle size is from 0.1 to
2.0fi inorganic or organic granules, liquid mineral oil, plasticizer, or liquid drying or non-drying animal or vegetable oil and fat with a surfactant added to the granules in an amount of about 0.5 to 40%; The mixture is preferably 1 to 15% so that the surface of the granules is sufficiently coated. Separately, predetermined amounts of agricultural chemicals and epidemic prevention chemicals are mixed with approximately the same amount of carrier such as clay, white carbon, etc.
It is produced by mixing it with powders such as silica frozen earth, bentonite, kaolin, talc, etc., or by mixing and pulverizing the mixture and coating the surface of the granular material. Furthermore, when the drug is a powder, the drug and carrier may be coated on the surface of the granules separately without being mixed in advance. Alternatively, it can also be produced by adding active ingredients to an oily substance containing a surfactant at room temperature or heating to make a liquid substance, which is then coated with talc or the like after absorbing the oil into base granules.
本発明に用いる農業用、防疫用薬剤は液状、粉末状の公
知の薬剤は何れも用いることができる。As the agricultural and epidemic prevention chemicals used in the present invention, any known liquid or powdered chemicals can be used.
以上の如くして得られた本発明の農業用防疫用粒状薬剤
は製造直後ですでに安定な被覆層の接着強度が得られ、
貯蔵経時期間中でも、その物理化学特性は酸化等の化学
的な変化を全くうけず、長期間安定性を保持することが
できる。The agricultural epidemic prevention granular drug of the present invention obtained as described above already has a stable adhesive strength of the coating layer immediately after production,
Even during storage, its physicochemical properties do not undergo any chemical changes such as oxidation, and it can maintain stability for a long period of time.
次に本発明の実施例を示す。Next, examples of the present invention will be shown.
実施例1
粒度0.5〜1.7鶴(32〜lOメ・ノシュ)の砕石
85部に機械油2.91部、ポリオキシエチレン(E、
02モル)ノニルフェニルエーテル0.045m、ポリ
オキシエチレン(E、05モル)ドデシルヘンゼンエー
テル0.03部及びドデシルベンゼンスルホン酸カルシ
ウム0.015部の混合物を攪拌しながら、あらかじめ
オリゼメート(3−アリルオキシ−1,2−ヘンジイソ
チアゾール−1,1−ジオキシド)8部、クレー8部を
混合粉砕した粉末16部を加えてオリ上メート8%粒剤
を得る。Example 1 85 parts of crushed stone with particle size of 0.5 to 1.7 Tsuru (32 to 10 Me Noche), 2.91 parts of machine oil, polyoxyethylene (E,
While stirring a mixture of 0.045 m of nonylphenyl ether (02 mol), 0.03 part of polyoxyethylene (E, 05 mol) dodecylhenzen ether, and 0.015 part of calcium dodecylbenzenesulfonate, 16 parts of a powder obtained by mixing and pulverizing 8 parts of -1,2-hendiisothiazole-1,1-dioxide) and 8 parts of clay are added to obtain 8% orimate granules.
実施例2
粒度0.5〜1.7m(32〜lOメソシユ)の砕石8
9部に機械油2.91部、ポリオキシエチレン(E、
02モル)ノニルフェニルエーテル0.045B、ポリ
オキシエチレン(E、05モル)ドデシルベンゼンエー
テル0.03部、ドデシルベンゼンスルホン酸カルシウ
ム0.015部を攪拌しながら加え、予めオリ上メート
4部、クレー4部を混合粉砕した粉末8部を前記の処理
を行った砕石粒に加え、被覆させてオリ上メート4%粒
剤を得る。Example 2 Crushed stone 8 with a particle size of 0.5 to 1.7 m (32 to 10 m)
9 parts, 2.91 parts of machine oil, polyoxyethylene (E,
0.02 mol) nonylphenyl ether, 0.03 part of polyoxyethylene (E, 0.5 mol) dodecylbenzene ether, and 0.015 part of calcium dodecylbenzenesulfonate were added with stirring, and 4 parts of ori-supermate and clay were added in advance. 8 parts of powder obtained by mixing and pulverizing 4 parts of the above-mentioned powder are added to the crushed stone grains subjected to the above treatment, and coated to obtain 4% orimate granules.
実施例3
粒度0.5〜1.7m(32〜IOメツシユ〉の海砂9
0部にポリエチレンオキシ(E、0=5) ドデシル
エーテル0.3部、スピンドル油1.7部を攪拌しなが
ら加え、更にマージエンド(2−クロロ−2′、6′−
ジエチル−N−ブトオキシメチルアセトアニリド) 5
部を加え、次にホワイトカーボン3部を粉衣してマージ
エンド5%粒剤を得る。Example 3 Sea sand 9 with a particle size of 0.5 to 1.7 m (32 to IO mesh)
To 0 parts, 0.3 parts of polyethyleneoxy (E, 0=5) dodecyl ether and 1.7 parts of spindle oil were added with stirring, and then merged end (2-chloro-2',6'-
diethyl-N-butoxymethylacetanilide) 5
1 part and then coated with 3 parts of white carbon to obtain a merged end 5% granule.
実施例4
粒度0.5〜1.7mm(32〜IOメツシユ)の汚砂
89部にナタネ油2.5部、ポリオキシエチレン(E、
04モル)オクチルフェニルエーテル0.5部を攪拌し
ながら加えて汚砂表面を湿潤させ、予めMIPC(2−
イソプロピルフェニル−N−メチルカーハフ−14部、
クレー4部を混合粉砕した粉体を加えて粉衣してMIP
C4%粒剤を得る。Example 4 2.5 parts of rapeseed oil, polyoxyethylene (E,
0.5 part of octylphenyl ether (04 mol) was added with stirring to moisten the surface of the polluted sand, and
14 parts of isopropylphenyl-N-methyl carhaf,
Mix and crush 4 parts of clay, add powder, coat with powder, and MIP.
C4% granules are obtained.
実施例5
粒径0.5〜0.8鴎の天然珪石(資)、5部に予めピ
リダフェンチオン(ジエチルオキソフエニルピリダジン
イルキスホロチオエ−日10部、落花生油7部、ポリオ
キシエチレン(E、08モル)オクチルフェニルエーテ
ル0.5部の混合物ヲ約(資)℃に加温熔融液を添加吸
油させ、後0.046m以下のホワイトカーボン2部を
粉衣させ防疫用ピリダフェンチオン10%粒剤を得る。Example 5 5 parts of natural silica stone with a particle size of 0.5 to 0.8, 10 parts of pyridafention (diethyloxophenylpyridazine ilkisholothioate), 7 parts of peanut oil, polyoxyethylene ( A mixture of 0.5 parts of octylphenyl ether (E, 08 mol) was heated to ℃ to absorb the oil, and then coated with 2 parts of white carbon of 0.046 m or less to form 10% grains of pyridafention for epidemic prevention. get the agent.
実施例6
粒径0.8〜1.6鶴の粒状尿素74.4部に予めミシ
ン油3.8部、ポリオキシエチレン(E、02モル)ノ
ニルフェニルエーテル0.1部、アラビアゴム0.1部
、水0.6部を混ぜたものを湿潤させる。Example 6 To 74.4 parts of granular urea having a particle size of 0.8 to 1.6 mm, 3.8 parts of sewing machine oil, 0.1 part of polyoxyethylene (E, 02 mol) nonylphenyl ether, and 0.5 parts of gum arabic were added. Moisten a mixture of 1 part and 0.6 parts of water.
これに更に予め2.4−ジクロロフェノキシ酢酸ナトリ
ウム7.5部、ベントナ412.5部、ホワイトカーボ
ン1部の混合粉砕粉体を加え粉衣して2.4−D ゛7
%粒剤を得る。To this, a mixed pulverized powder of 7.5 parts of sodium 2.4-dichlorophenoxyacetate, 412.5 parts of bentona, and 1 part of white carbon was added in advance and coated with powder to give 2.4-D゛7.
Obtain % granules.
次に本発明の粒状剤が従来の粒状剤に比べその優位性を
示す実験並びに評価を記す。Next, experiments and evaluations showing the superiority of the granules of the present invention over conventional granules will be described.
被覆法による粒状薬剤の製法において、本発明の被覆結
合剤を用いて製造した粒剤(本発明品)、従来用いられ
ている被覆結合剤である、ポリビニルアルコール、カル
ボキシメチルセルローズ等の水溶解性高分子化合物の水
溶液を被覆結合剤として用いた粒剤(対照例1)、エチ
レングリコール、ポリプロピレングリコール等の水溶性
脂肪族多価アルコールを被覆結合剤として用いた粒剤(
対照例2)、灯油、機械油を被覆結合剤として用いた粒
剤(対照例3)、天然動植物油特に乾性油を被覆結合剤
として用いた粒剤(対照例4)、合成乾性油を被覆結合
剤として用いた粒剤(対照例5)、合成樹脂粘着溶液を
被覆結合剤として用いた粒剤(対照例6)の粒剤につい
ての原料単価、製造エネルギー、貯蔵安定性、生物効果
についての評価を見れば次記第1表の通りである。In the method of manufacturing granular drugs by coating method, granules produced using the coating binder of the present invention (product of the present invention), water-soluble coating binders such as polyvinyl alcohol, carboxymethyl cellulose, etc., which are conventionally used coating binders. Granules using an aqueous solution of a polymer compound as a coating binder (Control Example 1); Granules using a water-soluble aliphatic polyhydric alcohol such as ethylene glycol or polypropylene glycol as a coating binder (
Comparative Example 2), Granules using kerosene or machine oil as a coating binder (Comparative Example 3), Granules using natural animal and vegetable oil, especially drying oil, as a coating binder (Comparative Example 4), Coating with synthetic drying oil Regarding the raw material unit price, manufacturing energy, storage stability, and biological effects of granules used as a binder (Control Example 5) and granules using a synthetic resin adhesive solution as a coating binder (Control Example 6), The evaluation is as shown in Table 1 below.
第1表
it)各評価面より最良のものを1とした時の各順位数
ここに貯蔵安定性の項に粉化とあるのは、製造直後では
みられぬが、一定時間経過後結合剤が硬化等を始めとす
る変化の為、部分的に硬化、収縮等が起り粒剤被覆層と
基粒間との接着強度の弱化する部分が露呈されるという
結果、粉化と言う現象を呈するのである。これに対し本
発明品は長期間安定性を期待出来る不乾性即ち飽和化合
物よりなる被覆接合剤を使用しているので製造直後です
でに安定な被覆層の接着強度が得られ、貯蔵経時期間中
でもその物理化学特性は酸化等の化学的な変化を全くう
けず、長期間安定性を保持出来る。Table 1 it) Each ranking number when the best one from each evaluation aspect is set as 1. Here, the term "powderization" in the storage stability section is not seen immediately after production, but after a certain period of time, the binder Due to changes such as hardening, partial hardening and shrinkage occur, exposing areas where the adhesive strength between the granule coating layer and the base grains is weakened, resulting in a phenomenon called powdering. It is. In contrast, the product of the present invention uses a non-drying coating bonding agent made of a saturated compound that can be expected to be stable for a long period of time, so the adhesive strength of the coating layer is already stable immediately after manufacturing, and even during storage. Its physicochemical properties are completely unaffected by chemical changes such as oxidation and can maintain stability for a long period of time.
又 対照例(2)のアルキレングリコール類を使用する
方法は本発明の被覆結合剤よりも蒸気圧が大きく、容器
の開封時には消失して粉化するおそれがある。又対照例
(3)は原料的には本発明品と同一素材を用いるが、界
面活性剤を含まず、その為に製造時のエネルギー、特に
造粒時間が長くかがり、又目的粒度域の粒剤製品の産量
も悪く施用後の生物効果発現の時間がおそく全体的な効
果が劣る。Furthermore, the method using alkylene glycols in Comparative Example (2) has a higher vapor pressure than the coated binder of the present invention, and there is a risk that it will disappear and turn into powder when the container is opened. Control example (3) uses the same material as the product of the present invention, but does not contain a surfactant, which requires energy during production, especially granulation time, and particles in the target particle size range. The yield of the product is also low, and the time required for biological effects to appear after application is slow, resulting in poor overall effectiveness.
又対照例!41. +5)は原則的に結合剤原料中に不
飽和結合を有する不飽和化合物を含む乾性油又は合成乾
性油を結合剤とするので、前記貯蔵中の酸化により、被
覆層の硬脆化が起り、この為粉化が起る。Another control example! 41. +5) basically uses a drying oil containing an unsaturated compound having an unsaturated bond in the binder raw material or a synthetic drying oil as a binder, so the coating layer becomes hard and brittle due to oxidation during storage. This causes powdering.
又、製造工程中、風乾又は加熱乾燥工程を要し、又これ
により出来た粒状薬剤は水中又は土壌水分に熔解又は分
散されることがな(水不溶性の為に施用後の薬剤の均一
分散が妨げられ効果発現の時間も長時間を要する。又対
照例(6)は他に比し一般に高価なものが多く又毒性も
大きい、又その接着強度も硬化剤を使用したり、高温で
焼付をして硬化させるもので特別の工程を要し、その樹
脂の耐候性を慎重に選択しなければ、農業用、防疫用薬
剤の有効成分の効果発現に至らぬ無能な粒剤を製造する
危険性がある。今これらの被覆結合剤を前記グループ別
のものとして、下記のものを選んで粒状農薬オリゼメー
ト8粒剤を試作した。In addition, during the manufacturing process, an air drying or heat drying process is required, and the resulting granular drug cannot be dissolved or dispersed in water or soil moisture (because it is water-insoluble, the drug cannot be uniformly dispersed after application). Comparative example (6) is generally more expensive and more toxic than others, and its adhesive strength is also limited by the use of hardening agents or baking at high temperatures. It requires a special process to harden, and if the weather resistance of the resin is not carefully selected, there is a risk of producing incompetent granules that do not exhibit the effects of the active ingredients of agricultural and epidemic prevention drugs. Now, among these coating binders according to the above-mentioned groups, the following were selected to make 8 granular agricultural chemical oryzemate granules.
被覆結合剤
本発明品
機械油、粘度詔、5センチボーズ 97部ポリオキシエ
チレン(E、04モル)ノニルフェニルエーテル
1.5部ポリオキシエチレン(E、06
モル)ドデシルエーテル
1.0部ドテシルヘンゼンスルホン酸カルシウム 0.
5部以上の混合液を本発明の被覆結合剤とした。Coating binder Inventive product Machine oil, viscosity, 5 cm Bose 97 parts Polyoxyethylene (E, 04 mol) Nonylphenyl ether
1.5 parts polyoxyethylene (E, 06
mole) dodecyl ether
1.0 parts Calcium dotesylhenzensulfonate 0.
A mixture of 5 parts or more was used as the coating binder of the present invention.
本発明の対照品の被覆結合剤として下記のものを用いた
。The following was used as a coating binder for a control product of the present invention.
対照例1 ポリビニルアルコール(鹸化度88モル)5
%水溶液
対照例2 ポリプロピレングリコール
対照例3 機械油(粘度 28.5センチポーズ (資
)°)対照例4 亜麻仁油
対照例5 ワニス
対照例6 尿素樹脂(65%固型分)
〔製法〕粒度0.5〜1.7鶴(32〜1oメソシユ)
の鉱物質砕石85部に上記被覆接合剤3部を平型攪拌機
に攪拌しながら加え全体を被覆接合剤でしめらしたのち
、予め、オリゼメート(資)%とクレー50%を混合粉
砕した製粉16部を粉衣被覆して製する。Control example 1 Polyvinyl alcohol (saponification degree 88 mol) 5
% aqueous solution control example 2 Polypropylene glycol control example 3 Machine oil (viscosity 28.5 centipose) control example 4 Linseed oil control example 5 Varnish control example 6 Urea resin (65% solids) [Manufacturing method] Particle size 0 .5 to 1.7 cranes (32 to 1 o mesosyu)
Add 3 parts of the above-mentioned coating binder to 85 parts of crushed mineral stone using a flat stirrer while stirring, and after soaking the whole with the coating binder, 16 parts of milled flour is prepared by mixing and pulverizing % Oryzemate (equipment) and 50% clay in advance. Manufactured by coating with powder.
但し本発明品、対照品の隘2及びN13以外の阻l。However, the products of the present invention and the control product had inhibitions other than No. 2 and N13.
lk4. N15及び陽6は1夜以上風乾して製した。lk4. N15 and Yo6 were made by air drying for over one night.
かくして製した稲熱病防除用オリ上メート8%粒剤0.
5〜1.70(32〜10メソシユ)粒度を有する製品
の収率及び製品の水中脱離度、加温虐待保存後の有効成
分の分解率及び粉化率を次の方法によって測定した。Orijomate 8% granules for controlling rice fever disease thus prepared 0.
The yield of a product having a particle size of 5 to 1.70 (32 to 10 mesos), the degree of desorption in water of the product, the decomposition rate and powdering rate of the active ingredient after storage under heating and abuse were measured by the following methods.
イ、水中脱離度
試料20gを精密に量り、標準硬水2oOmllを入れ
た共栓付250m1のメスシリンダーに加える。B. Accurately weigh 20g of the water desorption sample and add it to a 250ml graduated cylinder with a stopper containing 20Oml of standard hard water.
上下1回転を10秒の速さで5回転させた後、直ちに0
.15m (100メソシユ)のふるいを用いてふるい
つつ通過液を300mt!のビーカー中に移す。磁器攪
拌器を用いて液をかき混ぜながら、その50m1を正確
に300m/の分液漏斗に移し、100mIlのエーテ
ルで抽出する。水層は更に第2.第3の各分液漏斗に移
し、エーテルで抽出する。水層は捨てる。これらのエー
テル液を合わせ、無水硫酸ナトリウムを用いて親水後濾
過する。容器及び濾紙上の残留物は少量のエーテルで洗
い洗液は濾液に合わせ、エーテルを留去する。残留物に
アセトン10m1を加えてとかし、1mj!を薄層クロ
マトグラムプレートにスポットする。ベンゼン:アセト
ン 7:3混液で展開する。保持層比(Rf)約0.6
4のオリゼメート層をかきとリアセトン25m 12で
抽出する。この液5 m lに内部標準物質溶液(ジイ
ソブチルケトン0.3g/10mJ!アセトン)5mj
!を入れ、下記条件でガスクロマトグラフにかけオリゼ
メート量(Amg)を算出し次式により水中脱離度を算
出する。Immediately after 5 rotations of 1 rotation up and down at a speed of 10 seconds,
.. Using a 15m (100 mesh) sieve, 300mt of the liquid passed through the sieve! Transfer to a beaker. While stirring the liquid using a porcelain stirrer, 50 ml of it is accurately transferred to a 300 ml separatory funnel and extracted with 100 ml of ether. The aqueous layer is further divided into the second layer. Transfer to a third separatory funnel and extract with ether. Discard the water layer. These ether solutions are combined, hydrophilized using anhydrous sodium sulfate, and then filtered. The residue on the container and filter paper is washed with a small amount of ether, the washing liquid is combined with the filtrate, and the ether is distilled off. Add 10ml of acetone to the residue and dissolve it to make 1mj! Spot on a thin layer chromatogram plate. Develop with a 7:3 mixture of benzene:acetone. Retention layer ratio (Rf) approximately 0.6
Extract the oryzemate layer from Step 4 with oysters and 25ml of liacetone. Add 5 mj of internal standard substance solution (diisobutyl ketone 0.3 g/10 mJ! Acetone) to 5 ml of this solution.
! and subjected to gas chromatography under the following conditions to calculate the amount of oryzemate (Amg) and calculate the degree of desorption in water using the following formula.
オリゼメート R15,2分
内部標準物質 Rt 2.2分
試料20g中のオリゼメート量
(mg)
ガスクロマトグラフ操作条件
カラム担体;クロモソルブ W−AW DMC3液相
;5%シリコン OV −17
力ラム温度;21O。Oryzemate R15, 2 minutes Internal standard Rt 2.2 minutes Amount of oryzemate in 20 g of sample (mg) Gas chromatograph operating conditions Column carrier: Chromosolve W-AW DMC3 liquid phase: 5% silicon OV -17 Power ram temperature: 21O.
気化室;235゜
キャリヤガスiNz、50m#/分
検出器;水素炎イオン検出器 F、1.D口、有効成分
の残存率
製造当初のオリゼメート含量(g)に対する貯蔵経時後
の成分残存比(%)
但し、有効成分含量は試料5gをとり、アセトン10m
1で抽出し、上澄液1 m lを前記薄層クロマトグラ
フに分は以下同様に操作して算出する。Vaporization chamber; 235° carrier gas iNz, 50 m#/min detector; hydrogen flame ion detector F, 1. Port D: Remaining rate of active ingredient Ratio of remaining component after storage (%) to oryzemate content (g) at the time of manufacture.
1, and apply 1 ml of the supernatant liquid to the thin layer chromatograph described above.
検量線は予めオリゼメート純品を用し)で作成しておく
。A calibration curve was created in advance using pure Oryzemate.
ハ、 粉化率
試料100gをとり、内径100 vm、内部100m
mのボールミル磁製ボットに入れ、これに総重量105
gの直径約30鶴の磁製ボール3個を入れ、毎分75回
転で15分間回転した後、0.3鶴(48メ・ノシュ)
のふるいを通過した量の比率を粉化率とする。C. Take 100g of powdering rate sample, inner diameter 100vm, internal 100m.
m ball mill porcelain bot, and the total weight is 105.
Put 3 porcelain balls with a diameter of about 30 g and rotate at 75 revolutions per minute for 15 minutes, then 0.3 crane (48 me nosh)
The ratio of the amount passing through the sieve is the powdering rate.
これら特性値につき前記試作品の特性を検討して第2表
の結果を得た。The characteristics of the prototype were examined with respect to these characteristic values, and the results shown in Table 2 were obtained.
第2表
以上の如く、本発明の粒状薬剤は他に比し格段のすぐれ
た特性値を有する。As shown in Table 2 and above, the granular drug of the present invention has significantly superior characteristic values compared to others.
次に本発明の粒剤が従来の被覆結合剤を用いて製造され
た粒剤に比し、有効成分の効果の発揮がすぐれているこ
とを示す実験例をあげる。Next, we will give an experimental example showing that the granules of the present invention exhibit superior effects of the active ingredient compared to granules produced using conventional coated binders.
実験例1
供試粒剤
本発明品 実施例1のオリ上メート8%粒剤対照例1
実施例1の機械油、ポリオキシエチレンノニルフェニル
エーテル、ポリオキシエチレンドデシルベンゼンスルホ
ン酸カルシウム(以下、被覆結合剤と称す)の代りにカ
ルボオキシメチルセルローズ0.06部、水2.94部
(粘度700センチボーズ、鹸化値0.69)を用いた
他は実施例1と全く同様にして製造した粒剤
対照例2 実施例1の被覆結合剤の代りにポリプロピレ
ングリコール3部を用いた他は実施例1と全く同様にし
て製造した粒剤
対照例3 実施例1の被覆結合剤の代りにマシン油3部
を用いた他は実施例1と全く同様にして製造した粒剤
対照例4 実施例1の被覆結合剤の代りにアマニ油3部
を用いた他は実施例1と全く同様にして製造した粒剤
対照例5 実施例1の被覆結合剤の代りにワニス(固体
骨75%)4部を用いた他は実施例1と全く同様にして
製造した粒剤
対照例6 実施例1の被覆結合剤の代りに尿素樹脂(固
体骨ω%) 5部を用いた他は実施例1と全く同様にし
て製造した粒剤
水稲品種:ニシホマレ
挿挾月日二 6月詔日
収穫月日:10月31日
耕種概要:栽植密度、15 X 30cm (22,2
本/n?)施肥量:基油燐安280号(12−18−1
4)10a当り、40kg、追肥8月14日、8月27
日の2回同上肥料を10a当り20−夫々施用した。Experimental example 1 Test granules Present invention product Comparative example 1 of Example 1 8% granules
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity Granule control example 2, manufactured in exactly the same manner as in Example 1, except that 700 centiBose and saponification value of 0.69) were used. Granule control example 2, except that 3 parts of polypropylene glycol was used in place of the coating binder of Example 1. Granule Control Example 3 manufactured in exactly the same manner as in Example 1 Granule Control Example 4 manufactured in exactly the same manner as in Example 1 except that 3 parts of machine oil was used in place of the coating binder in Example 1 Granule control example 5 produced in exactly the same manner as in Example 1 except that 3 parts of linseed oil was used in place of the coating binder in Example 1. Varnish (75% solid bone) 4 in place of the coating binder in Example 1 Granule control example 6, manufactured in exactly the same manner as in Example 1, except that 5 parts of urea resin (solid bone ω%) was used instead of the coating binder of Example 1. Granular paddy rice variety produced in exactly the same way: Nishihomare Cutting date: June 2nd, Harvest date: October 31st Cultivation details: Planting density, 15 x 30 cm (22,2
Book/n? ) Fertilization amount: Base oil Rin'an No. 280 (12-18-1
4) 40kg per 10a, additional fertilizer August 14th, August 27th
The above fertilizer was applied twice a day at 20 doses per 10a.
区割面積:1凹面積10n?、各区波型畦畔板でかこっ
た。Divided area: 1 concave area 10n? , each area was surrounded by corrugated ridge boards.
散布月日及び散布量二8月13′F3に3 kg/ 1
0 aの量を散粒した。Spraying date and amount: 3 kg/1 on August 13'F3
An amount of 0 a was sprinkled.
調査月日、方法:いもち病発病調査は9月詔日各区父株
につき、枝梗いもち罹病程度1/3以上及び173以下
の発病穂率に分けて調査した。白葉枯病発病調査は9月
3日各区5株につき止5J30葉につき発病葉率及びそ
の病斑面積率を調査した。Survey date and method: The rice blast disease onset survey was carried out on father plants in each district on September's imperial edict, and was divided into the incidence of affected panicles of 1/3 or higher and 173 or lower. To investigate the onset of bacterial leaf blight, on September 3, the percentage of affected leaves and the percentage area of lesions were investigated for 5 J30 leaves of 5 plants in each section.
収量調査は10月31日収穫日に各区中心部3.3rr
r(73株)の精籾型(g)を調査した。The yield survey will be conducted on October 31st, the harvest day, at 3.3rr in the center of each district.
The spermatozoa type (g) of r (73 strains) was investigated.
調査成績を第3表で示す。The survey results are shown in Table 3.
第3表
実験例2
供試粒剤
本発明品 実施例2のオリゼメート4%粒剤対照例1
実施例2の機械油、ポリオキシエチレンノニルフェニル
エーテル、ポリオキシエチレンドデシルベンゼンスルホ
ン酸カルシウム(以下、被覆結合剤と称す)の代りにカ
ルボオキシメチルセルローズ0.06部、水2.94部
(粘度700センチポーズ、鹸化値0.69)を用いた
他は実施例2と全(同様にして製造した粒剤
対照例2 実施例2の被覆結合剤の代りにポリプロピレ
ングリコール3部を用いた他は実施例2と全く同様にし
て製造した粒剤
対照例3 実施例2の被覆結合剤の代りにマシン油3部
を用いた他は実施例2と全く同様にして製造した粒剤
対照例4 実施例2の被覆結合剤の代りにアマニ油3部
を用いた他は実施例2と全く同様にして製造した粒剤
対照例5 実施例2の被覆結合剤の代りにワニス(固体
分75%)4部を用いた他は実施例2と全く同様にして
製造した粒剤
対照例6 実施例2の被覆結合剤の代りに尿素樹脂(固
体分60%)5部を用いた他は実施例2と全く同様にし
て製造した粒剤
以上の各粒剤を実験例1と同様の水稲品種、挿挾月日、
収穫月日、耕種概要、区割面積、散布月日、散布量及び
調査月日、方法により穂首いもち、枝梗いもちの発病状
況を調査した結果を第4表に示す。Table 3 Experimental example 2 Test granules Present invention product Oryzemate 4% granules of Example 2 Control example 1
0.06 parts of carboxymethyl cellulose and 2.94 parts of water (viscosity 700 centipose, saponification value 0.69) was used (Granule control example 2 produced in the same manner as in Example 2) except that 3 parts of polypropylene glycol was used in place of the coating binder of Example 2. Granule control example 3 produced in exactly the same manner as in example 2 Granule control example 4 produced in exactly the same manner as in example 2 except that 3 parts of machine oil was used instead of the coating binder in example 2 Granule control example 5 produced in exactly the same manner as in Example 2, except that 3 parts of linseed oil was used instead of the coating binder of Example 2. Varnish (solid content 75%) was substituted for the coating binder of Example 2. Granule control example 6 produced in exactly the same manner as in Example 2 except that 4 parts were used. Example 2 except that 5 parts of urea resin (solid content 60%) was used instead of the coating binder of Example 2. Each of the granules manufactured in exactly the same manner as above was prepared using the same paddy rice variety, insertion date and date as in Experimental Example 1.
Table 4 shows the results of investigating the disease onset status of panicle neck blast and branch blast blast using harvest date, cultivation details, plot area, application date, application amount, survey date, and method.
第4表
以上の実験例1.2により明らかなように、本発明の粒
剤は従来の被覆結合剤を用いた粒剤に比し、オリゼメー
ト8%及び4%の農薬剤の効果がすくれている。As is clear from Experimental Example 1.2 in Table 4 and above, the granules of the present invention are less effective against pesticides containing 8% oryzemate and 4% compared to granules using conventional coated binders. ing.
実験例3
供試粒剤
本発明品 実施例3のマージエンド5%粒剤対照品
カオリン79.5部、ベントナイト20部、ドデシルベ
ンゼンスルホン酸ソーダ0.5部の混合粉体に水20部
を加えて捏造し押出造粒機にがけ、乾燥後0.5〜1.
7m (32〜10メツシユ)に篩分けて基粒を作る。Experimental Example 3 Test granule Inventive product Merged end 5% granule control product of Example 3
Add 20 parts of water to a mixed powder of 79.5 parts of kaolin, 20 parts of bentonite, and 0.5 parts of sodium dodecylbenzenesulfonate, make it, apply it to an extrusion granulator, and after drying, the powder will be 0.5-1.
Sieve into 7m (32 to 10 mesh) to form base grains.
これより95部をとり、攪拌しながらマーシェツト5部
を吸油したマーシェツト5%粒剤。From this, 95 parts were taken, and 5 parts of Marchet was absorbed while stirring to obtain a 5% Marchet granule.
水稲品種二M苗移植栽培ニシホマレ
播種月日: 5月28日、挿挾月日: 6月20日耕種
概要:栽植密度15 X 30cm (22,2本/r
rf)施肥量 基油硫安280号(12−18−4)1
0aあたり40kg施肥
区制面積:1区l〇−各区波型畦畔板でがこった。Paddy rice variety 2M seedling transplant cultivation Nishihomare Sowing date: May 28th, Insertion date: June 20th Cultivation details: Planting density 15 x 30cm (22.2 plants/r)
rf) Fertilization amount Base oil ammonium sulfate No. 280 (12-18-4) 1
Fertilization: 40kg per 0a Zone area: 1 zone 1〇 - Each zone was fertilized by corrugated ridge boards.
施用月日及び量、方法:挿侠前3日、挿挾直後及び3日
後の3時期に各々3kg/IOaの割合で土壌処理を行
った。Application date, amount, and method: Soil was treated at a rate of 3 kg/IOa at three times: 3 days before insertion, immediately after, and 3 days after insertion.
調査時期、方法ニア月加日揮挾初日後の各区雑草種別に
、雑草を抜き取り、水洗、風乾後の生体量(g)を秤量
した。Survey period and method: After the first day of weeding, weeds were pulled out from each area, washed with water, and the amount of living organisms (g) weighed after being air-dried.
調査結果を第5表に示す。The survey results are shown in Table 5.
第5表
以上の如く、本発明品は対照品よりも水田の一年生雑草
及び多年生雑草その他主要雑草の防除に効果があり、施
用時期も挿挾前3日〜当日迄の方が、挿挾3日後より効
果があった。As shown in Table 5, the product of the present invention is more effective than the control product in controlling annual weeds, perennial weeds, and other major weeds in paddy fields. It was more effective after a day.
実験例4
供試粒剤
本発明品、実施例4のMIPC4%粒剤対照品 汚砂8
7部に石炭酸樹脂系接着剤(固形公印%)5部を攪拌し
ながら加え、予めMIPC4部、クレー4部を混合粉砕
した粉体を加えて粉衣させ、65°±3℃で約2時間通
風乾燥させて得た粒剤
水稲品種:アソミノリ
挿秋月日= 6月20日
耕種概要:栽植密度15x3ocm基肥量塩加燐安28
0号(12−18−10> 10 a当り40kgm肥
、8月り6日塩加燐安280号10a当り20 kg
fF!肥区制面積:1区200rrf各区波型畦畔板で
かこった。Experimental Example 4 Test granules Invention product, MIPC 4% granule control product of Example 4 Dirty sand 8
Add 5 parts of carbonic acid resin adhesive (solid official stamp %) to 7 parts with stirring, add powder prepared by mixing and pulverizing 4 parts of MIPC and 4 parts of clay in advance, coat with powder, and heat at 65°±3°C for about 2 hours. Granules obtained by ventilation drying Paddy rice variety: Asominori Date of planting = June 20th Cultivation details: Planting density 15 x 3 occm Base fertilizer amount Salt and Phosphorus 28
No. 0 (12-18-10> 40 kgm fertilizer per 10 a, August 6th Shioka Rin-an No. 280 20 kg per 10 a
fF! Area covered by zoning: 200rrf per ward.Each ward is surrounded by corrugated ridge boards.
施用日時、量、方法二8月1日、102当り3kgの割
合で手撒き施用した。Date and time of application, amount and method: On August 1st, the application was carried out by hand at a rate of 3 kg per 102 cm.
調査時期及び方法ニア月31日(散布直前)8月20
(散布1日f&)8月15日(散布15日後)及び8月
30日(散布30日後)に次の掬い取り法及び払い落し
法により防虫効果を調査した。Survey timing and method Near August 31st (just before spraying) August 20th
(1st day of spraying f &) The insect repellent effect was investigated on August 15th (15 days after spraying) and August 30th (30 days after spraying) using the following scooping method and brushing off method.
掬い取り法:各区2プロットとして、口径36c11の
捕虫網を用いて各プロットより片振りで10回I20回
掬い取り、各区の害虫種別に計数した。Scooping method: Two plots were set in each plot, and insects were scooped 10 times and 20 times per plot using an insect trapping net with a diameter of 36c11, and each plot was counted according to pest type.
払い落し法;各区3プロットとして各プロ・/トから任
意に20株1θ0株を抽出し、粘着物を塗布した18
X 2Scn (B 5版大)の黒色セルロイド板に払
い落し害虫種類別に計数した。Brush-off method: 20 1θ0 plants were arbitrarily extracted from each plot as 3 plots in each plot, and adhesive was applied to them.
The pests were removed onto a black celluloid board of X2Scn (B5 size) and counted by type.
掬い取り調査の結果を次の第6表に、払い落し調査の結
果を第7表に示す。The results of the scooping survey are shown in Table 6 below, and the results of the scraping survey are shown in Table 7.
?!間昭58−124704 (19)第6表
第7表
以上の第6.第7表により明らかなように本発明品はヨ
コバイ、ウンカ類の防除に長期間にわたって効果があっ
た。? ! MaSho 58-124704 (19) Table 6, Table 7 and above. As is clear from Table 7, the product of the present invention was effective in controlling leafhoppers and planthoppers over a long period of time.
実験例5
供試粒剤 実施例5のlθ%ピリダフェンチオン粒剤
対照例 実施例5の組成のポリオキシエチレン(E、0
8モル)オクチルフェニルエーテル0.5部の代りに落
花生油 合計使用量7.5部を同様に操作して製造した
粒剤
以上の各粒剤をキンバエ最終令幼虫20匹 水10mj
2を入れた直径9cs高さ5cImの腰高シャーレに各
々1gを入れ一定時間後の殺岨力をみた結果を第8表に
示す。Experimental Example 5 Test Granules lθ% Pyridafention Granules Control Example of Example 5 Polyoxyethylene (E, 0
8 mol) Peanut oil in place of 0.5 part of octyl phenyl ether (Total amount used: 7.5 parts) Each granule prepared in the same manner was treated with 20 last instar fly larvae and 10 mj of water.
Table 8 shows the results of adding 1 g of each to a waist-height petri dish with a diameter of 9 c and a height of 5 c Im containing No. 2 and observing the killing power after a certain period of time.
第8表
殺姐率(%)
以上の結果より本発明粒剤は対照粒剤より殺岨力が速効
的にあられれる。Table 8: Killing rate (%) From the above results, the granules of the present invention exhibit more rapid killing power than the control granules.
特許出願人 三笠化学工業株式会社 代理人 伊東寸志(ばか2名)Patent applicant: Mikasa Chemical Industry Co., Ltd. Agent: Ito Sunshi (2 idiots)
Claims (1)
状の鉱物油、可塑剤又は液状の半乾性乃至不乾性の動植
物油脂に界面活性剤を加えた液状物を被覆し、その表面
に粉末状農業用防疫用薬剤を粉衣してなることを特徴と
する農業用防疫用粒状薬剤。1. Inorganic or organic granules with a particle size of 0.1 to 2.0 fi are coated with liquid mineral oil, a plasticizer, or a liquid mixture of semi-drying to non-drying animal and vegetable oils and fats with a surfactant added. A granular agent for agricultural epidemic prevention, characterized in that the surface thereof is coated with a powdered agricultural epidemic prevention agent.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP529682A JPS58124704A (en) | 1982-01-16 | 1982-01-16 | Granular chemical for agricultural and disinfection use |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP529682A JPS58124704A (en) | 1982-01-16 | 1982-01-16 | Granular chemical for agricultural and disinfection use |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS58124704A true JPS58124704A (en) | 1983-07-25 |
Family
ID=11607277
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP529682A Pending JPS58124704A (en) | 1982-01-16 | 1982-01-16 | Granular chemical for agricultural and disinfection use |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS58124704A (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61171402A (en) * | 1985-01-24 | 1986-08-02 | Takeda Chem Ind Ltd | Agricultural chemical preparation having reduced fish toxicity |
JPS6317802A (en) * | 1986-07-09 | 1988-01-25 | Mitsui Toatsu Chem Inc | Granular insecticide for application to water surface |
JPS63107902A (en) * | 1986-05-19 | 1988-05-12 | Takeda Chem Ind Ltd | Solid agricultural chemical formulation |
JPH08253401A (en) * | 1985-01-24 | 1996-10-01 | Takeda Chem Ind Ltd | Production in toxicity of agricultural chemical formulation against fish |
US10531661B2 (en) | 2016-02-16 | 2020-01-14 | Sumitomo Chemical Company, Limited | Coated agrochemical granule |
JP2021063024A (en) * | 2019-10-10 | 2021-04-22 | 竹本油脂株式会社 | Granulation improver for extrusion molding and method for producing agrochemical composition using the same |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS50140640A (en) * | 1974-04-29 | 1975-11-11 |
-
1982
- 1982-01-16 JP JP529682A patent/JPS58124704A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS50140640A (en) * | 1974-04-29 | 1975-11-11 |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61171402A (en) * | 1985-01-24 | 1986-08-02 | Takeda Chem Ind Ltd | Agricultural chemical preparation having reduced fish toxicity |
JPH08253401A (en) * | 1985-01-24 | 1996-10-01 | Takeda Chem Ind Ltd | Production in toxicity of agricultural chemical formulation against fish |
JPS63107902A (en) * | 1986-05-19 | 1988-05-12 | Takeda Chem Ind Ltd | Solid agricultural chemical formulation |
JP2551775B2 (en) * | 1986-05-19 | 1996-11-06 | 武田薬品工業株式会社 | Agrochemical solid formulation |
JPS6317802A (en) * | 1986-07-09 | 1988-01-25 | Mitsui Toatsu Chem Inc | Granular insecticide for application to water surface |
US10531661B2 (en) | 2016-02-16 | 2020-01-14 | Sumitomo Chemical Company, Limited | Coated agrochemical granule |
JP2021063024A (en) * | 2019-10-10 | 2021-04-22 | 竹本油脂株式会社 | Granulation improver for extrusion molding and method for producing agrochemical composition using the same |
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