PH26510A

PH26510A - Water-floatable aggregative solid agricultural preparations

Info

Publication number: PH26510A
Application number: PH39225A
Authority: PH
Inventors: Hisashi Obayashi; Tetsuo Okauchi; Norio Naito
Original assignee: Takeda Chemical Industries Ltd
Priority date: 1988-09-13
Filing date: 1989-09-13
Publication date: 1992-08-07
Also published as: KR0137493B1; KR900004251A; CN1041511A; CN1037484C

Description

Jud. 34570

BACKGROUND OF THE INVENTION

1. Field of the Invention

The pregent invention relates to water-float- sble, mggregative solid agricultural praparations, gspacially those containing carbamate agricultural chemicals and specific organic compounds. 2. Description of the Prior Art '

A yresearch is now being tried regarding the granular preparations which were glven a water-float- ability by coating or sbsorbing an insecticidal or like component with a water-floateble cerrier and coating the resultant with a water repallent, alter- natively by granulating a mixture of an insecticidal or like component and a carrier and coating the gra- nulgs with 8 water repellent. ;

For exemplas, Jespanese Patent Fublication No. 48(1973)-15613 discloses a floatsble grenular prepe- ration which wes mada by adsorbing an insecticidal component and a surfactant or water repellant on the base which was obtained by sticking and coating a submersible solid substance and a floateble substance together with a bindar, and Japenese Patent Publica tion No. 47(1972)-1240 discloses a floatable prepa- ration which binds an insecticidel component to a fat 26570 calcined perlite together with a polybutane. Japanes

Patent Publ ication No. 49(1974)-11421 discloses a granular preparation for paddy water application of an insecticidal compound which exerts an insecticidal effect by evaporating gas therefrom. This granular : preparation is obtained hy sticking fine powders, which are given water repellent properties by mixing a volatile insecticidal compound and a water repel- lent with or without a carrier, to the surface of a granular base.

Moreover, Japanese Patent Publication No. 44(1969)-8600 discloses a floatable granular insecti- cidal composition prepared by adsorbing an active " component on granular pumice or vermiculite having 30-50% of water-absorbability as carrier and costing the resultant with a higher fatty acid. oo

However, all of the prior art references stated } above require the use of the water-floatable carrier [Japanese Patent Publication Nos. 48(1973) - 15613 and 47(1972) - 12407 or the carrier of pumice or vermiculite having a specified water-absorbability . [Japanese Patent Publication No. 44(1969) - 8600, or are limited to the granular preperat ions which utilize the volatile insecticidal component (Japanese

Patent Publication No. 49(1974)-11421). Or, they show a drawback of not in practical use because said preparation have very complexed composition. Moreover, ~ while these preparations have a merit to reduce -3 a= " i fod. 24510 parts to be wasted because of adsorption by soil or dissolution to the bottom waster due to their floatasion whan they are esppliad to paddy water as granular pre- parations, they have still disadvantages that soma parts of them d o not well coms into contact with plente and are wasted beacause the actives component scatters to a whole water surface or 1s less adhe- rency to plants,

The inventions of the present invention aimed to find an agricultural preparation that when it is subjected to paddy water application, an active in- gredient can coma into contact with a plant effective- ly end sscend the surface of stem due to the phano- menon of capillarity or stick directly to leaf end gtem of plant, thersby giving a high control efficacy around the plant stock base region or plant foot.

SUMMARY OF THE INVENTION

Thus, tha inventions have unexpectedly found : that carbsmate agricultursl chemicals have s desirable spreadehility on e water surface (harainaf ter called as "spredability"), UWhan this sprdfadebility of car- bemate agricultural chemicals is utilized, 1t wes also found that active ingradients including other insecticides or fungicides are simultaneously spread

Jit 268 10 end aggregated or accumulated around water surface at a high concentration. Accordingly, when pre- parations containing carbamate agricultural chemicals are subjected to paddy water application, active in- gredients can be spread and aggregated sround weter surface at a high concentration, and hence can be well adhered to the stem and leaf. It wes also found that when an organic compound having the partition cosfficient of the agricultural chemical to water of not leas than 102 was eddsd to the sbove prasparation, 1% gnebled to more effectively aggregate active in- gradients eround weter surface and maintain them at = high concentration and for a longer period of time.

According to the present invention, it pro- vides 8 water-flostebls, aggregative solid agricul- tural preperation which comprises garrying (1) a car- bamata egricultural chemical es the active ingredient (1) end (2) an orgenic compound (II) having a perti- tion coefficient of sald carbamate agricultural che mical (I) to water of not less then 102, on (3) a so- 1id cerrier, end optionally conteining a thiolcar- bemats insecticide such ss cartep”hydroochloride /T,3- bia(carbamoyl-thin)=2=(N,N-dimathylamino)~propans hydrochloridg/ or bensultep/5,5'-/Z~(dimethylemino)- trimethylena/bis(benzenathiosulfonate)/.

ff. 246/0

PREFERRED EMBODIMENTS OF THE INVENTION

The carbamate agricultural chemicals (I) to bs employad in this invention, mey be eny carbamate type insecticide or fungicide having spreadebility and aggregative sbility on water surface. Prefersble examplas of ths carbsmate egricultursl chemicels (I) are compounds rapresentasd by the following formula:

R=NHCOD- Ay (1) - wherein R 1s a lower alkyl group end Ar is a phanyl : 1d or naphthyl group optionally having a substituent,

Exemplas of the lower alkyl group represented by R in the formula (I') are alkyl groups having 1 to 6 carbons such as methyl, ethyl, propyl, isopropyl, butyl, pentyl and hexyl, Substituents on the phanyl or naphthyl group represented by Ar may bs such lower alkyl group as examplified before in R, a halogen such es chlorine or bromine and an alkoxy Hroup having 1 to 6 carbons,

Specifically, the carbemate sgricultural che- micals (I) mey be BPMC (O-amec-butylphenyl mathylcer- bamate), MIPC (2-1sopropylphenyl-N-methylcarbemste),

NAC (l-naphthyl-N-methylearbemate )y, XMC (3,5exylyle

Nemethylcarbamate) and MTMC (m=-tolyl-N-mathylcarba- mate), to which they are not limited. The carbemate fae

Spurl CIA -8~

Jad. 26510 sgrioulfral chemicals (IX) are sided usually in about © 30 = 0.3 parts by weight, preferably about 10 - 2 parte ty weight, relative $0 100 parts by weight of the total preparetion,

The preparation ef the present invention msy op- tionally combein other agricultural chemicals then. the above mentioned carbamate agricultural chemioals (I) oY

Their preferable exsmples are insecticides or fungieides 40 be used for plant food appliestiom; Specifieslly, ¥hiolecarbumate insecticides such sv cartsp hytrechleride or bensultap are conveniently sided *hen oexrtsp hydrochloride or benmultep having mm exosllant effect en a rice borer is sided, he preparation em be utilised oe a controlling egent agwinet a ew : pL lesthopper,

Remples of other usable agrioultirel chemiesls to be incorporatel in the preperstion are insecticides such : os MEP /5,0-dinethyl O-(4-nitro-m=tolyl Wii ephonphats/, &eminon J5,0-d1etly) O-(t-dveproryl-i-metiyl-bupyrinityl}= intophoesiuta), tecxeition 5,0 ety O-(3-sheny1-s 480xesol Wiiophosphiuta/) malethon J5-(1y 2-24 emrbethany- ottyL) O,0-dimetbyl ditttophoaphiat/ ad a pyrettrold in secticide, or fungicides such ee validsmyeins; These sgrietltural chenicals may be aided singly ow in mixture 1] thereof, wl usually sdded in about Ol « 15 parts YW -T= "BAD ORIGINAL

Jif 26510 weight, prefersbly 0,2 = 5 parts by weight, to 100 paris by weight of the preparation, she orgenie compound (I1), mother indispensable element of the present invention means, those having a

S partition coefficient of the exrbamate motive ingredient : "{X) %0 water of no less than 10%, The compound (II) hev- ing no sgrioultural setivityy but having a high bolling point 4s usually used. The compound (IT) which is liquid ; at ordinary teaperature (unless explieitly mentioned, the ordingry teaperatures means 15% hereunder) is preferred,

In the present invention, the partition ecefficient is she partition coefficient ordinarily used es a measure ofs liporhilie property, It means the constant in the partition law mentioned on page 209 of Encyclopedia :

Ohimdes Vol, 8, (edited by Encyclopedia Ohbmica Editor's

Committee, Kyoritsu Mmppen, Jepmn, 1962); Namely, the . partition law 4s defined in the Fwpxlopedia Chimice os "When a third material (solute) 4s dissolved in two oo 1iquids which are substentislly imsiscitle essh other and when dhey are cosxisting, the conoemiration ratis in 4hese two liquids becomes constant st a fixed Sempersture oo regardless of the comsentretion”s The constant value in the partition law is called partition coefficient, Nw

Wari tion cosffiotemt® in the yresent invention mews alvo the partition coefficient wo defined Tn the present —8- BAD ORIGINAL fat. 6518 invention, the two liquids correspond to the water in paddy. fields and the organic compound (II), snd the solute corresponds to the active ingredient (1). By taking the concentration of the active ingredient (1) in the organic compound (I1) at ordinary temperature as "Co" and the concentration of the active ingre~ - dient (I) in water as "Cw", the partition coefficient can be represented by Co/Cw. Namely the orgenic com- pound (II) in the present invention means those suf- ficing the equation of Co/Cw : 10°. Although there is no upper limit of the partition coefficient Co/Cw of the organic compound (II) in the present inven- tion, it is preferred to be no more than 107.

Summarizingly, the preferred condition of the organic compound (II) is 102 4 Co/Cw { 107 (at or- . ginary temperature. More preferred condition is 10° ¢ Co/Cw $108 (at ordnary temperature). The ordinary temperature means 15°C in this case, too.

Among the organic compounds (11) having a partie tion coeffieient to the active ingredient (I) of no "less than 102, preferably no more than 107, the come pounds in liquid at ordinary temperature and sufficing the following conditions are preferred onest (1) the solubility to water at ordinary temperature 28 ie no more than 5% (by weight). . (414) boiling point is no lower than 160°C. (411) it dissolves no less than 1% (by weight of the = °° -9 - " oo

Jat 26570 © askive ingredient (I) ob ardinary temperature;

As the organie compounds (II) sufficing the sbove mentioned gonditions, the followings are exemplified: (2) fatty acid esters having the following foxwmla s (111) to

R00, © wherein I represents a siraight or branehsd alkyl : N : &roup of Og po, or an alkenyl group of Op and By represents a straight or Wranched alkyl group of (11) dtesters having the following formula (IV): 00, | - (omy go, * wherein Ry represents a siraight or tranched alkyl group of Op and m represents sn integer of 2-4, 1 (111) phosphates having $he following formula (v) . BO :

Ry0 peo

Cu wherein R,, Ry, and Rg wre seme or different smd re-

Cee | lao ORIGINAL I

' ’ - TT - 1(1I14) PTVE0Z SUTMOTIOS OGY Bupa Segsosusq (TA) 1

Co todvoxd Og pw Bg

SETETIINS JO Jaquet oy Fuuonm C-T eusem b pus d Tp 30 drosk TAYE pepwem Io VETS § 0 } woss ueloxpixy © sueseadex OF pus 6 By yreaeua . : by’ . a¢8x) , . { oT, Co : ot wh (11a) VTMNIOZ SutuoTyes uy Supany seuvqyewr mgd Tp (4) tadvoxs by STON TROqVE mqwm oqy Fupaoys pt suwem w 9135 30 anoxs

TAXTe pea 20 yFPeays © syusesadex Ly upexerm uly) 7

TE TV Id SupmoTToF oY Futawy seussueqTA(Te ( A¥)

Sdnoxs hued » 2 TY) 0 dwoad pore pessutsoTye 8 CTE 30 dnox® Tire peyowwaq Jo yudtenys © quesexd sK fo ] oo = BAD ORIGINAL

Val 24519 wherein Ryy represents a straight or twsnched al-

W1 group of 0; (vid) phthalate having to following foormla (x),

COOR, 5 <r wherein each of R,, and Riy represents a straight md branched alkyl group of Oy.39°

Preferable exsuples of the alkyl group of 0p yy in By of the fatty acid ester (111) are Gyo alkyl groupe oo such as nonyl, undeayl, trideayl, pentsiesyl, heptedecyl,

Preferable exemples of the alkenyl groups of Op.04 in By are Oy 49 alkenyl groups such o» oleyl LB p, Cnech(oH, Je! or lnoleyl [OK Oe0H(0R, Mle Preferably, the 0, ., allyl groups of R, may be Oy o alkyl groups such o8 dutyl, 1s ‘axyl, hexyl or heptyl, Specific exmtple of the fatty aid enters (III) are mmyl lmirate; amyl myristate, butyl pudmitate, amyl palmitate, hexyl palmitate, butyl stearste, myl stearate, hexyl stearate, Mutyl oleste, amyl oleate oo - iP = i

LEE

Tro BAD ORIGINAL

Jat. 250 sod butyl linolate.

Preferably examples of the Opq2 alkyl groups in By of the desters (IV) wre Cp, ligl groups meh on ethyl, propyl, butyl, mmyl, hexyl, heptyl and ootyl. s Specifically, the diesters (IV) may be diethyl succinate, dipromyl succinate, ditutyl, socinste, dimyl sugoinste, d1o0kyl succinate, diethyl ghrismate, dibutyl ghutemste, dimyl glutamate, diootyl glutmate, dibutyl sdipate, diay) atipate or dioetyl siipatee

Preferable examples of the Oy ,, s1kyl groups in (Ryy By, end Rg) of the phosphate (V) are 0,5 oiy2 groups such ss butyl, smyl, hexyl or ootyl. In the same stricture, the 0, chlorinated sligl groups (Ryo Rg Rg) sre preferably 0, chlorinated alkyl groups mich as ri- 13 chlorosthyl ar triehléroproryl: Ascardingly, the phee- phate esters (V) nay be tribukyl phosphate, trimgl phos phate, trioceiyl phosphate, butyl diphenyl phosphate, oolyl di7henyl phosphate or tri(chloroethyl) phosphate! } © Preferable exemples of the 0, yg sliyl groups (ry) of the alkylbensens (VI) are Op go SUNy1 groups such os ethyl, mwopyl, isopropyl, tyl, teobutyl, seo-buiyl, tert-butyl, amyl, 1somyl, Sert-myls ool or decyls

The compounds (VI) are thoes having 14 seme or diffevent : substituents mentioned above on the bensens ring. “. 28 Spesifie exsaples of the alkylbensenes (V1) wre divthyl- “ld =

- (of. p45 benzene, diisopropylbenzene, triisopropylbenzene, tert-butylbenzene, di(tert-butyl)benzene, diamylben- } gene, triamylbenzene, tetraamylbenzene, tert-amylben~ zene, di(tert-amyl)benzene, octylbenzene, dodecylben- ot gene and didodecylbenzene,

Examples of the Cy.3 alkyl groups (Rg, Rg Co

Ro? of the diphenylmethanes (VIII) are methyl, é thyl, . propyl or isopropyl. When the diphenylmethane (VII) has two or three of Rg having a C13 alkyl group, these Cy.3 alkyl groups may be the same or different. } Similarly, in case where the diphenylmethane (VII) has two or three of Rg having a Cy3 alkyl, they ney be the same or different. Accordingly, the di=- : : ; phenylmethane (VII) is exemplified by phenylxylyl- : ethene, phenylxylylpropane, trixylylethane, dixylyl- ) methane and diisoxylylethane. : - The Cy.12 alkyl groups (R14) of the benzoate vIn are preferably C, _g alkyl groups such as me- . “thyl, ethyl, butyl, amyl, hexyl or octyl. Specifical- . 20 ly, the benzoate (VIII) may be methyl benzoate, ethyl - benzoate, butyl benzoate, amyl benzoate, hexyl benzo-

Co - ate, octyl benzoate or nonyl benzoate. . | The C,_,, alkyl groups (Ry, R),) of the : phthalate (IX) are preferably C, g alkyl groups such as methyl, ethyl, butyl, amyl, hexyl or octyl. Speci= ‘ficelly, the phthalate (IX) may be dimethyl phthalate, : : diethyl phthalate, dibutyl phthalate or dioctyl phthale - ll = :

Jat 5) ate.

The org:nic compounds (II) may be used sing- ly or in mixture thereof.

The organic compounds (II) are usually used oy 5 in about 5 - 0.1 parte by weight, preferably about 3 - 0.2 parts by weight, to one part by weight of ths carbamate type active ingredient (I).

Any solid carriers which are ahle to give a water-floatability to the preperation can be used as the carriers of this invention. The solid cerrisrs having 8 particle diamater of 60 - 1000 pm ars gena- rally preferable. The use of the solid carrier having @ particle diameter of less then 60 od is not desire sable generally becauss of safaty and hygienic issues and difficulty in due to & whirling of powders. The use of the solid carrier having a particle diesmeter of more than 1000 pm is also not deasireble because of the low drying efficiency dus to floatahility and epread- bility of the ;reparetion on s water surface although #8 whirling of powders can be suppressed completasly,

More preferable particls diameter of the carrier is in Tree ths range of 100 -~ B00 um, Exemples of tha solid care riers are those having watsr-floatability in theme salves;, such as perlite, vermiculite, pumice /=.g. 2% Klite No. 3(R) (KANSAI JARI KK)7, walnut powder obe oo Ff. 2ts10 teinable by pulverizing the shell of a welnut, or woodan powder, and also those which sink per sa but becoma water-floatshle by ® combination use with a water repellant, such as crushed or otherwise come minuted sand product (hersinafter sometimes refarred to briefly ms crushed sand) /e.g. those disclosed in

Jepanass Unexamined Publicstion No. (1986) - 2863027, silica sand /B.g. river sand (Hayashi Kasei, Japan)7, rhyolite fe.g. Hinoyalite (Hinaya Shokei, Japen),

Kagalite (Tango Kensetsu, Japan)/, granular diatomite [=-0. Carstom'R) (Kakiuchi Shoji, Jepen)7, and other water soluble grenuler mineral carriers with particle diameter of 60 - 1000 um such as granular ammonium sul fate or grenulsr urea, Among these garriers, perlite mesns a produgt prepared from obsidian, perlite or othar vitreous volcanic rocks which swsll by heating, and is commercially avallsble with various grades,

Examples of commercial products of perlites sre Topuko #34,

Topuko®Y #54, Topuke® 4/71 /Bvatlebls from Toko

Perlite Hogyo Co., Ltd. Japap/ and Perlite Meigara types 1 [Available from Ube Industries, Ltd, Japan/. Vermi- culite hag the structures like Mg (54, A1)0(0HIMg. H,0 and is svailable with various grades with or without palcination, Walnut flour /Nippon walnut Co., Ltd. dapon/ is exemplified se a commercial product of tha fad 54570 walnut powder. Even in case of the aforesaid solid carriers having specific gravity of more then 1, they become water-floateble by the combination with a water repellent, magnesium stearate or the like,

As such solid are conveniently used crushed sand, prefershly crushed sand with a particle diamater of 60 - 1000 pm (which is Bvailsbls by crushing more finely sccording to the method disclosed in the Jape nese Unexamined Patent Putlication No, 61(1986)- 286302, and pumice, Farticularly praferred are crushed sand of perticle diameter of 60 - 1000 pme

The solid carriers having a preferable particls dia- meter of 60 - 1000 um are eassily availabla from the market. It is also possible to obtaln $he carriers having a desired particle diesmaeter by sizing or screening using conventional vibratory filtration or cyclone method, Besides, basalt, andssite, sendatons, ‘quartz porphyry end those having a stone quality aimiler thereto sre used as the crushed sand men=- tioned above. Such raw pre can be pulvarized after removing top soil and other impurities by using, for example, scarping screen, ripple “flow screen end ths like. A similar process to the manufacture of grinded bone materials is utilized in reducing a raw ore ine 23 to powdsr., A grinded powder of a rew ore 1s obtained,

fed. 02510 for example, at first by getting rid of surfacs soll and other impurities, and then grinding them gredusl- dy by using known grindars in order, for mxampla, Jou crusher (crusher for crushing 8 big lump), cohan

S grusher for crushing a madium size lump) and impera bresker (crusher for getting fina pieces), and there- after classifying them by elr separator.

Thoss solid cerriers which are able to give 8 floatebility to the preperation are usually used in about 30 - 98 weight parts, preferably 63 = 93 waight parte, to 100 weight prts of the total preperation.

However, it is also possible, if desired, to usa, in addition to the solid carriers mentioned above which are appropriate to give a floetsbility to the pre- peraticns, one or more kinds of other solid carriers such ss vegetable powders, clays, telcs, silicas (diatomite, etc.), zeolite, river sand, calcium cer- 'bonate and the like, in an extent of not disturbing the effect of this invention. In this invention, it is desirable to mix thoroughly the carbamate agricul- tural chemicel end, if desired, tha other active com- ponent, with the aforesaid solid carriers snd more prefarsbly to make the sctive components adhere to or adsorb in the solid carriers or to coat the solid carriers with the active componenta. In order to im-

Jed 2570 prove sdhsrsnce of those components, it is possibls to add a conventional binding agent, such as sodium varboxymethylcellulose (CMC-Na), polyvinyl alcohol, starch, polyoxyethylena waxes (s.g. polyoxyethylena- nonylphenylsthar, polyoxysthylens glycol, atc.) and the like, When a water repellent of this invention, such as hydrophobic esrosil /&.g. neros11®?) n-972 (Nippon Aercsil KK)/, magnesium stearate, purified talc, silicon oil and the like 1s added to the pre- paration, it is effective to prolong the floatsbility of the preparation and also to give floatability to she solid carrier with a specific gravity of more than 1, TThe amount of the water repellent is usual- ly sbout 0.05 ~ 5 weight parts, prefarably 0.1 - 2 weight perts, to 100 weight parts of the preparation.

CL It is \lso possible to edd a higher fatty acld dn order to improve water repasllent properties and/ or water-floatebility of the praparstions, Preferable sxemples of the higher fatty acids era those having 8 to 20 carbons, mapecielly such es stearic acid, pele mitic acid end lsuric acid. These fatty acids can ba used singly or in mixturs thereof. If need ba, it ie alao possible to edd, a surfectent (s.g. polyoxyaty- ranephenol), and an sntioxidant (e.g. isopropyl ecid 235 phosphate), a flow suxiliasry agsnt, a8 lubricant, a

(od 26572 stabilizer (e.g. phosphosic ecid, tartaric scid, stc.) stc. to an extent that the effect of this invention is not disturbed,

The preparation of this invention can be manufactured by mixing the cerbamate sgricultural chemical (I) and the orgenic compound (II) with thas solid carrier in accordance with the conventionel mathod. It 1s preferable, by mixing tham thoroughly to meke the ective component adhere to or edsurb in the solid carrier or to cost the solid carrier with the active component. In the mixing process the car- bamate agricultural chamical (I) end optionally the pther active componenta are usually edded to the so- 14d carrier in a conventional mixer, such as drum type mixer, and then mixed by further edding the eforementioned organic compound (II) heving a perti- tion coefficient of not less then 102, Altarnetive- ly, it is also possible to mix first the carrier and the binding agent snd then to add the main active in- gradient thereto in order to adheres it to ths carrier pr to coat the cerrier with it. In such way, the ordar of the mixing is not limited. ’

The preparations sra desirable to ba manuface tured as granular preparations in sccordance with the gonventional method. However, it is also possible to - 20 - So fod D6588 prepare them as fine granules, subtilized granulas or powdery granules, which have more fine particles,

In prepering the granular prepsrations, the conventional method can be used, for example, such as the wet granulation method which follows the pro=- cesses of addition of weter, kneading, granulating end drying, after mixing in the miser such es the aforesaid drum-type mixer.

The dosage of the agricultural preparation of this invention varies, depending upon plece, timing and method of application, tergeted blights, crops, etc, However, it is generally about 0.85 - 50 g, pre- ferably 2 - 20 g, more preferably 8 - 16 g par one ars of a paddy field as the active componasnts cone tainad therein, inclusive of the carbamate agricul- tural chemicsl and the optionel other sctivas com- panent.

Thig invention ip further illuatrstad by exam ples and test sxamples,

In the following examples, "part" means "part by weight",

Examples 1

A homogeneous mixturs of 3,0 parts of BPMC and 2.0 parts of octyldiphsnylphosphate (hereinafter i (at 75 abbreviated a ODP) was poured into 54,8 parts of pumice having a perticle diameter of 300 - 600 um in @ drum mixer under rotating, to carry the mixture Te on pumice, 0.2 part of magnesium stearate (abbreviated as St-Mg) to the resultant were added to obtain ths guated granuler preparation.

Exemple 2

A homogenous: mixturs of 4.0 parts of MIPC and 4,0 parts of dioctyl adipate (abbreviated as DOA) was poured into 93.0 parts of Kagalite having a perticle diameter of 100 - 500 um in a drum mixture under rotat- ing, to carry the mixturs on Kagalits, follousd by addition of 1.0 part of purified talc. Thus the coated granular preparation was obtained,

Exempla 3

A homogenous , mixtura of 4.0 perts of BPMC and 4.0 parts of ODP was poured into 86.6 parta of cenaron@® having 8 particle diameter of 300 = 700 pm in a drum mixer under rotating, to carry the mixture on CERATUM, followed by eddition of 4,0 parts of cer- tep hydrochloride (abbreviated gs CT) and 1.2 parts of FEG-400. Then, 0.2 pert of nerostL ® R=-972 ware mixad with the resultant to obtain the costed grenular preperation.

. : Example k

A homogenous mixture of 4.0 parts of MIPC and 4.0 parts of ODP was poured into 86.2 parts of CERAe rouE in a drum mixer under rorating followed by - addition of 4.0 part of BENSULTAP and 1.2 parts of

PEG-200. Then, 0.3 part of St-Mg were mixed with the resultant to obtain the coated granular preparation. -

Example 9 "© A homogeneuss mixture of 2.5 parts of NAC and 1.5 parts of diethyl phthalate was poured with 92.5 parts of granular ammonium sulfate in a drum mixer under rotating, followed by addition of 2 parts of bensultap. Then 1.5 parts of purified talc were . mixed with the resultant to obtain the coated granular ‘ 15 preparation.

Example 6 , A homogenous mixture of 4.0 parts of BPMC and 4,0 parts of ODP was poured into 86.8 parts of CERA- ’ rol® having a particle dismeter of 150 - 550 pe in sa drum mixer under rotating, followed by addition of 4.0 parts of CT and 1.0 part of walidemycin A. Then, 0.2 part of AEROSIL® R-972 were mixed vith the re- sultant to obtain the granular preparation.

fit 74538

Example 7

A homogenous mixture of 4,0 parts of HIPC and oo ) 4.0 parts of DOA was poured into 86.0 parts of Hino- yalite in a drums mixer under rotating, followed by addition of 4.0 parts of bensultap and 1.5 parts of : validemycin A. Then, 0.5 part of St-Mg were well mixed with the resultant to obtain the granular pre- paration. : Example 8 - 10 A homogenous mixture of 2.0 parts of BPMO and 1.0 parts of diethyl phthalate was poured into 95.8 parts of granular ures in Nauta mixer under rotating, followed by addition of 0s5 parts of velidamycin A. ’ Further, 0.3 part of silicon oil and O.4 part of white carbon were added to obtain the granular pre« --paration. . Example 9 ‘

A homogenous mixture of 3.0 parts of BPMC, 5.0 "parts of ethyl bensoate and 3.0 parts of MEP vas added to 88.7 parts of cxraron® having a particle diameter of 250 = 600 po in Nauta mixer under rotate ; "ing, followed by well mixing with 0.3 part of acros1L® R=972 to obtain the coated granular pre= paration. ee eo 2b »

vo fil. 7510

Example 10 - In a rotating drum mixer, 4.0 parts of BPMC - and 4.0 parts of ODP were added to 86.3 parts of curator ®) having a particle diameter of 300 - 700 pas followed by addition of 1.5 parts of poly= ‘ethylenenonylphenylether. Then, 0.2 part of asros LP

R-972 were mixed with the resultant to obtain the gra- nular preparation. .

Example 11

To 89.25 parts of pumice having a particle diameter of 300 - 500 pe in a drummini xer was poured a homogenous mixture of 4.0 parts of melted BPMC, 2.0 parts of DOA and 0.25 part of isopropyl acid phosphate,

After mixing, 4.0 parts of CT were added to the ree sultant mixture, followed by addition of 0.5 part of ako ILD R-972 to obtain the coated granular prepa- oo ration.

The following is the examples of the control preparations which do not belong to this invention.

Control Preparation 1 (corresponding to Example 3) 4.0 Parts of ODP, 4.0 parts of ‘CT, 0.2 part of apros1L 1-972 and 1.2 parts of PEG-400 were added to 77.6 parte of clay, which were thoroughly mixed in a drum mixer. To the resultant mixture were fur=- ther added 12 parts of water, kneaded, granulated and fod. 26510 dried to obtain the preparation having a particle - : diame ter of 800 poe

Control Preparation 2 (corresponding to Example h4) : 4.0 Parts of ODP, h.0 parts of bensultap, 1.5 parts of PEG-200 and 0.3 parts of 8t-Mg were added to 79.2 parts of clay, which were thoroughly in a drum mixer. Further, 12 parts of water were added to the mixture, kneaded, granulated and dried to ob- tain the preparation having a particle diameter of 500 p=. a

Control Preparation 3 (corresponding to Example 9) 3 Parts of MEP, 5 parts of benzyl alcohol and 0.3 part of aeros1L® R972 were added to 79.2 parts of olay, which were thoroughly mixed in Nauta mixer.

To the resultant mixture were added 12.5 parts of. water, kneaded, granulated and dried to obtain the . - granular preparation having a particle diameter of 200 pee - | oo

Efficacy test against Nilaparvata lugens 2k « 30 pimagos of female Nilaparvata lugens vere released for 5 - 6 days on 22 days (repeat 1) - 29 days (repeat 2) before application of the drug preparation in a large greenhouse made by noryl resin to give an oviposition onto rice plant (species:

Nippon bare, stage of growth at the time when the - 26 - BAD ORIGINAL —— ee of HED drug was applied: optimum fillering stage, culti- vation density: 20 sthmps,/n°) transplanted to the bed (1 m x 1 m) in said green house. A specified amount of each of the aforesaid preparations was sprayed equally by hand onto the rice plant with the target to the insects mainly consisting of lar- ’ vee of the next generation stemming from said ovi- position.

The number of surviving insects on the 4 stumps at the center of the bed was counted on the dey before application of the preparation and each of the one and three days after application of the preparation, and the efficacy of the drugs was evaluated : in terms of an average by determining the corrected re- : 15 production index in accordance with the following fore : pulat C.R.I. (Corrected Reproduction Index): 100 x (X1/X0)/(Ci/Co) wherein Xi and Xo mean the numbers of surviving insects at each drug application area on one day after the application, respectively, and Ci and Co mean the numbers of surviving insects at non- drug application area on one day after the drug appli- cation and on the dey before the drug application, ' . respectively. The corrected reproduction index 100 indicates that no efficacy of the preparation was ob- served. eo 27 »

/ / LL 7 rE fle

Results of Efficacy Test against Nilaparvata lugens

EE ET

® ' Control nN

Preparation 1 33.4 : Control '

Preparation 2 19.9 2h.0

CD ee we

Control to

Preparation 4 18.5%

Te ee [ee

Note: The efficacy of the drug is indicated by the corrected reproduction index (CRI) (average of 2 repeats). ait indicates the amount of the pure active substance.

BA 26530 © Efficacy test sgainst Pellicularia sasakii . . 40 mg of the preparation was sown equally by : hand on the rice plant (speciest Shinsenbon, stage oo of growth at the time when the preparation was applied: 8 - 9 weeks) transplanted into pot (1/10,000 a), on which Pellicularia sasakii was inoculated.

Those treated with the preparation one day after inoculation oo . is referred to as the cure test and those treated with : : the preparation 1 hour after inoculation is referred © 10 : to as the prophylactic test. ~~ oo The efficacy was determined by measuring the : distance from the soil surface of the rice plant up to top of the disease pungtum at 10 days after in- : fection. . a .

: , NT

Jal 26518

Table

Results of Efficacy Test against Pellicularia sasakii

The preparations Prophylactic Effect Cure Effect : (cm) (cm)

The granular preparation of Example 6 1,52

The granular preparation of Exemple 7 1.18 : . The granular preparation of Example 8 0.01 1.04

The control preparation } 1 15.98 Co 19.66

The control preparation oo 4 10.67 16.07 ! . . ea 30 e

Claims

J - : : - Ad est oo WHAT WE CLAIM ISt l.
A water-floatable, aggregative solid : agricultural composition which comprises carrying i (1) a carbamate agricultural chemical having Co the formula of R-NHCOO-Ar wherein R is a lower alkyl group and Ar ie a phenyl or naphthyl group which may K : be “subst itted by the group consisting of an alkyl :
i. ) group having 1 to 6 carbon atoms, a halogen and an . alkoxy group having 1 to 6 carbon atoms and having : 10 ' spreadabllity and aggregative ability on water sure . face as the active ingredient, {n an amount of 0.5- 30 parts by weight relative to 100 parts by weight of the total composition and oo © (2) an organic compound having & partition soefficlent of said carbamate agricultural chemical SE | (1) to water of not less than 10%, a solubility to Co water at ordinary temperature which is no more than 5% : “hy weight), a property which can disdolve fot less ‘then 1% (by weight) of said carbamate agricultural | chemical, no agricultural activity and a litgh boiling oo CC point which is not lower than 160°C and being liquid : at ordinary temperature, in an amount of 0.1 = 5 parts by weight to one part by weight of said carbamdte agri~ : : : Co } cultural chemical, on (3) a aolid carriers - 3 | Sm a
4, A composition of Claim 1 which further contains validamycin A.
5. A composition of Claim 1 in whicl the so- 1id carrier has a particle diameter of 60 =, 1000 pee
6. A composition of Cleim 1 in which the so- © 14d carrier is a crushed sand having a particle dime meter of 60 - 1000 pa. | : :
4 7. A composition of Claim 1 which further contains a water repellent.
8. A composition of Claim 2 which further oo contains validamycin A. : : : 94 A composition of Claim 2 which further "* contains a water repellent. : Le HISASHI OBAYASHI TETSUO. OKAUCHI - NORIO NAITO oo . Inventors : . od i . -o