DK155771B - PROCEDURE FOR THE PREPARATION OF DUST-FREE PLANT PROTECTIVE GRANULATES - Google Patents
PROCEDURE FOR THE PREPARATION OF DUST-FREE PLANT PROTECTIVE GRANULATES Download PDFInfo
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- DK155771B DK155771B DK040679AA DK40679A DK155771B DK 155771 B DK155771 B DK 155771B DK 040679A A DK040679A A DK 040679AA DK 40679 A DK40679 A DK 40679A DK 155771 B DK155771 B DK 155771B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/12—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic in rotating drums
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
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Description
DK 155771 BDK 155771 B
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Den foreliggende opfindelse angår en hidtil ukendt fremgangsmåde til fremstilling af støvfrie plantebeskyttelsesmiddel- granulater.The present invention relates to a novel process for the preparation of dust-free plant protection granules.
Fremstillingen o$ anvendelsen af granulerede plante-5 beskyttelsesmidler har længe været kendt [jvf. Martin, The Scientific Principles of Crop Protection (1959), 5. oplag, og van Valkenburg, Pesticide Formulation (1973)]. Blandt de forskellige tekniske muligheder for fremstilling af plantebeskyttelsesmiddel-granulater indtager fremgangsmåder, ved 10 hvilke i forvejen fremstillede gfanulater eller kernematerialer, der består af naturlige, uorganiske eller organiske eller syntetiske bærestoffer, omhylles med lag indeholdende aktiv forbindelse, en særlig stilling (jvf. van Valkenburg, Pesticide Formulation (1973), US-PS nr. 3.849.105, CA-PS 15 nr. 714.528, GB-PS nr. 815.829 og DE-PS nr. 1.199.049). Ved omhylning af et bærergranulat opnås nemlig en kontrollerbar rådighed over den aktive forbindelse, der befinder sig i om-hylningen, og som kun påvirkes lidt af kernematerialets egenskaber.The preparation and use of granulated plant protection products has long been known [cf. Martin, The Scientific Principles of Crop Protection (1959), 5th Edition, and van Valkenburg, Pesticide Formulation (1973)]. Among the various technical options for the preparation of plant protection product granules, processes in which pre-made gfanulates or core materials consisting of natural, inorganic or organic or synthetic carriers occupy layers with active compound layers have a special position (cf. van Valkenburg, Pesticide Formulation (1973), U.S. Patent No. 3,849,105, CA-PS 15 No. 714,528, GB-PS No. 815,829, and DE-PS No. 1,199,049). Namely, by wrapping a carrier granule a controllable availability of the active compound contained in the sheath is obtained which is only slightly affected by the properties of the core material.
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Ved disse i forvejen beskrevne fremgangsmåder kan omhylningslagene påføres de i forvejen fremstillede bærermaterialer på meget forskellig måde. Det er f.eks. således kendt at frembringe omhylningslaget ved hjælp af den klæbende forbindelse mellem et pulver (findelt faststof) og en lidet flyg-25 tig olie, hvorved såvel pulveret (det findelte faststof) som olien kan være det biologisk aktive princip. Plantebeskyttelsesmiddel-granulater, der fremstilles ved disse i forvejen kendte fremgangsmåder, kan ganske vist fremstilles med en relativ ringe indsats med hensyn til apparater og omkostnin-30 ger, men de har ikke altid tilfredsstillende egenskaber til anvendelsen. På grund af den uregelsmæssige overflade af sådanne granulater dannes der således en større eller mindre mængde støv ved afgnidning ved håndtering og transport af dem. For brugeren af plantebeskyttelsesmiddel-granulater 35 betyder støvet en sundhedsfare. Derudover optræder der uøn-In these previously described methods, the coating layers can be applied to the pre-fabricated carrier materials in very different ways. It is e.g. thus known to produce the envelope layer by the adhesive connection between a powder (finely divided solid) and a little volatile oil, whereby both the powder (the finely divided solid) and the oil can be the biologically active principle. Plant protection product granules prepared by these methods known in the art can be produced with relatively little effort in terms of apparatus and cost, but they do not always have satisfactory properties for use. Thus, due to the irregular surface of such granules, a greater or lesser amount of dust is formed upon abrasion when handling and transporting them. For the user of plant protection product granules 35, the dust poses a health hazard. In addition, undesirable
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2 skede afdriftssymptomer ved påføringen af sådanne støvholdige granulater. Derved går ikke blot en del af den aktive forbindelse tabt for det i forvejen fastsatte anvendelsesområde, men der kan også - først og fremmest ved påføring af her-5 bicid-granulater - opstå skader i kulturer, der er naboer til anvendelsesområdet.2, there were symptoms of drift when applying such dusty granules. This not only loses part of the active compound for its predetermined scope, but also - first and foremost when application of herbicidal granules - can result in damage to cultures that are neighbors to the field of application.
Det er endvidere kendt at frembringe plantebeskyttelsesmiddel-granulater med et omhylningslag, der er mere modstandsdygtigt mod afgnidning ved, at man i stedet for pul-10 ver-olie-systemet påfører vandige eller organiske opløsninger eller emulsioner (latexer) af naturlige eller syntetiske polymere, hvilke opløsninger eller emulsioner indeholder aktiv forbindelse, på de i forvejen fremstillede bærermaterialer (jvf. CA-PS nr. 714.528 og CH-PS nr. 473.742). Det er imidler-15 tid en ulempe ved fremstillingen af sådanne granulater, at der næppe kan undgås en relativ høj maskinel indsats. Fremgangsmåden kræver således en totrinsproces, der gennemføres i successivt anvendte apparater (maskiner). Det første trin er fremstillingen af omhylningslaget, der fortrinsvis sker i blande-20 apparater. Det andet trin er en tørre- eller reaktionsproces, der gennemføres i tromletørrere, rørtørrere, vakuumtørrere, tør- «** rere for fluidiseret masse og andre tørreapparater (jvf. van Val-kenburg, Pesticide Formulation (1973), Sherrington, The Chemical Engineer ^6, Nr. 220 (1968), 201 - 215, og Sherrington, 25 The Canadian Journal of Chemical Engineering Vol. 47 (1969), 308/316). Det er endvidere en ulempe ved de på denne måde fremstillede plantebeskyttelsesmiddel-granulater, at den afgnidningsbetingede støvdannelse heller ikke her kan hindres i tilstrækkelig grad.Furthermore, it is known to produce plant protection product granules with a coating layer that is more resistant to abrasion by applying aqueous or organic solutions or emulsions (latexes) of natural or synthetic polymers instead of the powder-oil system. which solutions or emulsions contain active compound on the already prepared carrier materials (cf. CA-PS No. 714,528 and CH-PS No. 473,742). However, it is a disadvantage in the manufacture of such granules that a relatively high mechanical effort can hardly be avoided. Thus, the process requires a two-step process carried out in successively used appliances (machines). The first step is the preparation of the casing layer, which preferably takes place in mixing apparatus. The second step is a drying or reaction process carried out in drum dryers, pipe dryers, vacuum dryers, fluid mass dryers and other dryers (cf. van Valkenburg, Pesticide Formulation (1973), Sherrington, The Chemical Engineer ^ 6, No. 220 (1968), 201-215, and Sherrington, 25 The Canadian Journal of Chemical Engineering Vol. 47 (1969), 308/316). Furthermore, it is a disadvantage of the plant protection product granules produced in this way that the abrasion-dependent dust formation cannot be sufficiently prevented here as well.
30 Det har nu vist sig, at der kan fremstilles støvfrie plantebeskyttelsesmiddel-granulater, ved en fremgangsmåde, som er ejendommelig ved, at man a) i et åbent blandeapparat, hvis omdrejningsretning eventuelt kan anvendes om, først anbringer bærermateriale 35 (kernemateriale), b) dernæst under blanding tilsætter bindemiddel og30 It has now been found that dust-free plant protection granules can be produced by a process which is characterized in that a) in an open mixer whose direction of rotation can possibly be used, first apply carrier material 35 (core material), b ) then, during mixing, add binder and
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3 omhylningsmateriale, der kan indeholde op til 100% plantebeskyttelsesmiddel, samt eventuelt tilsætningssstoffer og c) dernæst under gastilførsel tørrer i det åbne blan-deapparat, hvis omdrejningsretning eventuelt kan vendes om.3 wrapping material which may contain up to 100% plant protection agent, as well as any additives; and c) then, during gas supply, dries in the open mixing apparatus, the direction of rotation of which may be reversed.
5 Man har endvidere fundet frem til, at den her om handlede fremgangsmåde til fremstilling af støvfrie plantebeskyttelsesmiddel-granulater hensigtsmæssigt gennemføres ved hjælp af et i den ene eller i begge sider åbent blande-apparat, hvis omdrejningsretning eventuelt kan vendes om, 10 og som har tilførselsorganer for bærergranulat, findelte faststoffer og gas.It has further been found that the method of the present invention for the preparation of dust-free pesticide granules is conveniently carried out by means of a mixing apparatus open in one or both sides, the direction of rotation of which may be reversed, 10 and which has carrier granule feedstock, finely divided solids and gas.
Det må betegnes som yderst overraskende, at der ved den her omhandlede fremgangsmåde kan fremstilles støvfrie plantebeskyttelsesmiddel-granulater i et åbent blandeapparat, 15 hvis omdrejningsretning eventuelt kan vendes om, thi på grund af teknikkens kendte stade måtte det antages, at der ved arbejde ved en sådan enkeltbeholderfremgangsmåde ville optræde en agglomerering, dvs. en sammenklumpning af de løse granulat-masser. I modsætning til forventningerne er dette imidlertid 20 ikke tilfældet. Det er endvidere overraskende, at en forstyrrelsesfri tørring af granulatet i det åbne blandeapparat er mulig ved den her omhandlede fremgangsmåde, selvom den løse granulatmasse i skarp modsætning til konventionelle tørrere ikke foreligger i tynd, men i høj lagtykkelse.It is to be considered extremely surprising that the process of the present invention can produce dust-free plant protection granules in an open mixer whose direction of rotation can possibly be reversed, because, because of the known state of the art, such single container method would occur agglomeration, i.e. an aggregation of the loose granular masses. However, contrary to expectations, this is not the case. Furthermore, it is surprising that an interference-free drying of the granulate in the open mixer is possible in the process of the present invention, although the loose granulate mass is not in sharp contrast to conventional dryers, but in high layer thickness.
25 Den her omhandlede fremgangsmåde har en række fordele.25 The present process has a number of advantages.
Der kræves således kun en relativ ringe apparatindsats, fordi granulatfremstilling og tørring gennemføres i samme apparat.Thus, only a relatively small apparatus effort is required, because granulation and drying are carried out in the same apparatus.
Der kræves endvidere mindre energi end ved tilsvarende traditionelle fremgangsmåder, fordi en del af den til tørringen af 30 granulatet nødvendige energi tilvejebringes ved gnidningsvarme i den løse granulatmasse. En anden væsentlig fordel ved den her omhandlede fremgangsmåde består i, at de fremkomne granulater har en glat overflade og dermed også en højere modstandsevne mod afgnidning. Dette betyder, at der på den ene side 35 næsten ikke dannes støv ved fremstillingen af granulatet, på grund af hvilket støv betjeningspersonalet kunne udsættes forFurthermore, less energy is required than by similar conventional methods, because part of the energy needed for drying the granulate is provided by rubbing heat in the loose granular mass. Another significant advantage of the present process is that the resulting granules have a smooth surface and thus also a higher abrasion resistance. This means that on the one hand 35, hardly any dust is formed in the preparation of the granulate, due to which dust the operating personnel could be exposed to
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fare. På den anden side optræder der heller ingen uønskede afdriftssymptomer ved påføringen af granulaterne. Endelig er den her omhandlede fremgangsmåde også egnet til fremstilling af granulater, der indeholder temperaturfølsomme forbindelser, 5 der er aktive som plantebeskyttelsesmidler, fordi de temperaturer, der er nødvendige til tørringen af produkterne, ligger forholdsmæssigt lavt. Den her omhandlede fremgangsmåde udgør således en værdifuld berigelse af teknikken.danger. On the other hand, no undesirable drift symptoms occur when applying the granules. Finally, the present process is also suitable for the preparation of granules containing temperature-sensitive compounds which are active as plant protection agents because the temperatures required for drying the products are relatively low. Thus, the present process constitutes a valuable enrichment of the technique.
Som bærermaterialer (kernematerialer) kan der ved gennemførelsen af den her omhandlede fremgangsmåde anvendes alle gængse, finkornede faststoffer, der kommer på tale til fremstillingen af granulater. Til disse hører fortrinsvis brudte og fraktionerede, naturlige stenmelarter, såsom calcit, marmor, kvartssand, pimpsten, sepiolith og dolomit, endvidere 15 syntetiske forbindelser ud fra uorganiske og organiske, findelte materialer samt desuden findelte materialer ud fra organisk materiale, såsom savsmuld, kokosnøddeskaller, majskolber og tobaksstængler.As the carrier materials (core materials), all common, fine-grained solids which are involved in the preparation of granules can be used in carrying out the process of the present invention. These include, preferably, broken and fractionated natural rock melts such as calcite, marble, quartz sand, pumice, sepiolith and dolomite, as well as synthetic compounds from inorganic and organic, finely divided materials as well as finely divided materials from organic material such as sawdust, coconut shells, corn cobs and tobacco stalks.
2Q Som bindemiddel kan der ved gennemførelsen af den her omhandlede fremgangsmåde anvendes alle bindemidler {adhæsiver) , der er gængse til fremstilingen af granulater. Til disse hører fortrinsvis opløsninger, emulsioner eller latexer af naturlige eller syntetiske, organiske forbindelser, såsom 25 methylcellulose, dextrin, stivelse, polyvinylpyrrolidon, lig-ninsulfonat, gummi arabicum, polyvinylalkohol og polyvinyl-acetat, i vand eller i lavtkogende, organiske opløsningsmidler, såsom methanol, ethanol, butanol og methylenchlorid.2Q As a binder, in the process of the present process, all binders (adhesives) common to the manufacture of granules can be used. Preferably, these include solutions, emulsions or latexes of natural or synthetic organic compounds such as methyl cellulose, dextrin, starch, polyvinylpyrrolidone, lignin sulfonate, gum arabic, polyvinyl alcohol and polyvinyl acetate, in water or in low boiling, organic methanol, ethanol, butanol and methylene chloride.
På tale som omhylningsmaterialer ved gennemførelsen 30 af den her omhandlede fremgangsmåde kommer alle stoffer, der er gængse til granulatfremstiliingen. Således kan omhylnings-materialet fortrinsvis bestå af en eller flere, som plantebeskyttelsesmiddel aktive forbindelser. Som omhylningsmate-riale kan fortrinsvis også anvendes blandinger af en eller 35 flere, som plantebeskyttelsesmiddel aktive forbindelser samt fyldmaterialer, emulgatorer, dispergeringsmidler, klæbemidlerSpeaking as wrapping materials in carrying out the process of this invention, all substances common to the granule preparation come. Thus, the wrapping material may preferably consist of one or more active compounds as a plant protection agent. Preferably, as a coating material, mixtures of one or more active compounds as plant protection agents and fillers, emulsifiers, dispersants, adhesives can also be used.
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og/eller farvestoffer. På tale som fyldmaterialer kommer her uorganiske eller organiske, faste bærerstoffer, såsom naturlige stenmelarter, f.eks. kaoliner, lerjordarter, talkum, kridt, kvarts, attapulgit, montmorillonit eller diatoméjord, 5 endvidere syntetiske stenmelarter, såsom højdispers kiselsyre, aluminiumoxid og silicater, og endvidere findelte materialer af naturlige, organiske forbindelser, såsom fint savsmuld, korkmel og tobaksstøv. På tale som emulgatorer kommer ikke--ionogene og anioniske emulgatorer, såsom polyoxyethylen-10 fedtsyreestere, polyoxyethylenfedtalkoholethere, f.eks. alkylarylpolyglycolether, alkylsulfonater, alkylsulfater samt proteinhydrolysater. Som dispergeringsmidler kan der anvendes ligninsulfonater og methylcellulose. På tale som klæbemidler kommer sådanne bindemidler, som allerede er 15 nævnt i foregående afsnit. Som farvestoffer kan fortrinsvis anvendes uorganiske pigmenter, såsom jernoxid, titandioxid og ferrocyanblåt, eller organiske farvestoffer, såsom alizarin-, azo- og metalphthalocyaninfarvestoffer.and / or dyes. Speaking as fillers, here come inorganic or organic solid carriers, such as natural stone melts, e.g. kaolinens, clay soils, talc, chalk, quartz, attapulgite, montmorillonite or diatomaceous earth, 5 addition, synthetic stone flour, such as high-dispersion silicic acid, alumina and silicates, and also finely divided materials of natural organic compounds such as fine sawdust, cork flour and tobacco powder. Speaking as emulsifiers come nonionic and anionic emulsifiers such as polyoxyethylene fatty acid esters, polyoxyethylene fatty alcohol ethers, e.g. alkylaryl polyglycol ether, alkyl sulfonates, alkyl sulfates and protein hydrolysates. As dispersants, lignin sulfonates and methyl cellulose can be used. Speaking as adhesives comes such binders, already mentioned 15 in the previous section. Inorganic pigments such as iron oxide, titanium dioxide and ferrocyan blue, or organic dyes such as alizarin, azo and metal phthalocyanine dyes, may preferably be used as dyes.
Som forbindelser, der er aktive som plantebeskyttel- 20 sesmidler, kan der ved gennemførelsen af den her omhandlede fremgangsmåde anvendes alle aktive forbindelser, der kan påføres i forvejen fremstillede bærermaterialer, såsom insekticider, nematodicider, fungicider og herbicider. Som eksempel skal nævnes: 25 3-(3,4-dichlorphenyl)-1,1-dimethylurinståf, 3-sek.butyl-5-brom-6-methyluracil, 3-amino-l,2,4-triazol, hexahydro-lH-azepin-l-carbamidsyre-thiolester, 0,0-diethyl-S-(2-ethylmercaptoethyl)-dithio-phosphorsyreester, 30 2,2-dimethyl-2,3-dihydrobenzofuranyl-7-methylcarbamat, 2-i sopropoxypheny1-N-methy1carbamat, 2-(ethylthiomethyl-phenyl)-N-methylcarbamat, 0-ethyl-0-(3-methyl-4-methylthio-phenyl)-isopropylamidophos- 35 Phat °« 2,4-dichlorphenoxy-propionsyresalte.As compounds which are active as plant protection agents, all active compounds which can be applied to pre-prepared carrier materials such as insecticides, nematodicides, fungicides and herbicides can be used in the practice of the present invention. By way of example: 3- (3,4-dichlorophenyl) -1,1-dimethylurea, 3-sec-butyl-5-bromo-6-methyluracil, 3-amino-1,2,4-triazole, hexahydroxyl 1H-azepine-1-carbamic acid thiol ester, 0.0-diethyl S- (2-ethylmercaptoethyl) -dithiophosphoric ester, 2,2-dimethyl-2,3-dihydrobenzofuranyl-7-methylcarbamate, 2-i sopropoxyphenyl N-methylcarbamate, 2- (ethylthiomethyl-phenyl) -N-methylcarbamate, 0-ethyl-0- (3-methyl-4-methylthio-phenyl) -isopropylamidophosphate-2,4-dichlorophenoxy-propionic acid salts.
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6 På tale som tilsætningsstoffer, der kan anvendes ved gennemførelsen af den her omhandlede fremgangsmåde, kommer alle tilsætningsstoffer, der er gængse til granulatfremstilling.6 Speaking as additives which can be used in carrying out the process of this invention, all additives common to granule preparation come.
Til disse hører f.eks. coating-opløsninger, dvs. opløsninger, 5 der er egnede til at frembringe et yderligere lag på granulatpartiklerne. Sådanne coating-opløsninger er f.eks. vandige poly-vinylacetatopløsninger eller vandige urinstof-formaldehyd-op-løsninger, der også kan indeholde citronsyre eller andre katalysatorer til accelerering af kondensationen.These include e.g. coating solutions, i.e. solutions suitable for producing an additional layer on the granular particles. Such coating solutions are e.g. aqueous polyvinyl acetate solutions or aqueous urea-formaldehyde solutions which may also contain citric acid or other catalysts to accelerate the condensation.
10 I den sidste fase af den her omhandlede fremgangs måde sker tørringen af granulatet ved anvendelse af gasser med forhøjet temperatur og lav mætningsgrad af vanddamp eller opløsningsmiddel. Via gasstrømmen reguleres temperaturen på den løse granulatmasse og den relative mætning af luftrummet 15 i blandeapparatet med vanddamp og/eller opløsningsmiddeldamp således, at en kondensering og derved en agglomeratdannelse forhindres. I overensstemmelse hermed skal den minimale gasmængde og dens temperatur være udmålt således, at ingen dampkondensering er mulig. Ved denne type tørring tilvejebringes 20 en væsentlig andel af den til tørringen nødvendige energi af den gnidningsvarme, der opstår i den løse granulatmasse under blandingen.In the final phase of the process of the present invention, the drying of the granulate is effected using gases of elevated temperature and low saturation of water vapor or solvent. Via the gas stream, the temperature of the loose granulate mass and the relative saturation of the air space 15 in the mixer are regulated with water vapor and / or solvent vapor so as to prevent condensation and thereby an agglomerate formation. Accordingly, the minimum gas quantity and its temperature must be metered so that no vapor condensation is possible. In this type of drying, 20 provides a substantial portion of the energy needed for drying the heat of rubbing generated in the loose granular mass during mixing.
te Tørrevarigheden kan varieres inden for et større område. Den ligger almindeligvis på mellem 5 minutter og 25 2 timer, fortrinsvis på mellem 10 minutter og 1 time.The drying duration can be varied within a larger area. It is usually between 5 minutes and 2 hours, preferably between 10 minutes and 1 hour.
Hvis man anvender et blandeapparat, der er åbent i den ene side, tilledes den regulerbare gasstrøm til tørringen af granulatet gennem blandeåpparatets chargeringsåbning. Ved anvendelse af et blandeapparat, der er åbent i begge sider, 30 gennemledes eller gennemsuges den regulerbare gasstrøm gennem blandeapparatet.If one mixer open on one side is used, the adjustable gas flow is allowed to dry the granulate through the mixer opening port. By using a mixer open on both sides, the adjustable gas flow through or through the mixer is passed or suctioned.
Som gasser til tørringen kan der især anvendes luft, nitrogen eller forbrændingsgasser. Gasstrømmens temperatur kan varieres inden for et større område, afhængigt af granulatet.In particular, as gases for the drying, air, nitrogen or combustion gases can be used. The temperature of the gas stream can be varied within a larger range, depending on the granulate.
35 Gasstrømmens tilgangstemperatur ligger almindeligvis på under 100°C, fortrinsvis mellem 50 og 80°C.The inlet temperature of the gas stream is generally below 100 ° C, preferably between 50 and 80 ° C.
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Apparatet til gennemførelse af den her omhandlede fremgangsmåde består af et i den ene eller i begge sider åbent blandeapparat, hvis omdrejningsretning eventuelt kan vendes om, og som har tilførselsorganer for bærergranulat, findelte fast-5 stoffer, der anvendes som omhylningsmateriale, bindemiddel og gas.The apparatus for carrying out the process of the present invention consists of a mixer open in one or both sides, the direction of rotation of which may be reversed, and which has feed granular supply means, finely divided solids used as a coating material, binder and gas.
Som blandeapparat kan der her anvendes alle i den ene eller i begge sider åbne blandeapparater, hvis omdrejningsretning eventuelt kan ændres under driften. Blandeapparater 10 af denne type er kendt fra byggeindustrien eller fra den kemiske apparatteknik. Det er særlig fordelagtigt at anvende et i begge sider åbent blandeapparat, hvis blandekedel er usymmetrisk opbygget. Ved et sådant blandeapparat har chargeringssiden stejle vægge, medens fraføringssiden er konisk 15 udformet. De indbyggede hjælpeorganer til bevægelse og gennem-blanding af den løse granulatmasse er anordnet således, at de i den ene omdrejningsretning kun har en ringe aksial trans-portvirkningsgrad i retning af chargeringsåbningen, medens de efter vending af omdrejningsretningen hurtigt transporte-20 rer granulatet gennem fraføringsåbningen.As a mixer, all mixers open in one or both sides may be used here, the direction of rotation which may be changed during operation. Mixers 10 of this type are known from the construction industry or from the chemical apparatus technique. It is particularly advantageous to use a mixer open on both sides whose mixing boiler is asymmetrically constructed. In such a mixer, the charging side has steep walls, while the discharge side is conically shaped. The built-in auxiliary means for moving and blending the loose granular mass are arranged so that in one direction of rotation they have only a small axial transport efficiency in the direction of the charging opening, while after reversing the direction of rotation the granulate is rapidly transported through the discharge opening. .
På tale som tilførselsorganer for bærergranulat (kernemateriale) kortimer sådanne gængse løfte- og vippeapparater, som er kendt ved byggemaskiner og anlæg i den kemiske industri.Speaking as carrier granular feedstock (core material), such common lifting and tilting devices are known to cure, as is known by construction machinery and plants in the chemical industry.
På tale som tilførselsorganer for bindemidler, dvs.Speaking as delivery agents for binders, ie.
25 vandige eller organiske opløsninger eller emulsioner, kommer simple dyser. Sidstnævnte er fortrinsvis anbragt kun et lille stykke over granulatmassen i blandeapparatet.25 aqueous or organic solutions or emulsions come simple nozzles. The latter is preferably located only a short distance above the granular mass in the mixer.
På tale som tilførselsorganer for findelte faststoffer, der anvendes som omhylningsmateriale, kommer gængse ΟΛ transportsnekker. Transportsnekkerne er her indbygget på en sådan måde i blandeapparatet, at deres åbning ligeledes er anbragt kun et lille .stykke over granulatmassen.Speaking as feedstock for finely divided solids used as wrapping material, common n transport carpets come. The conveyors are here incorporated in such a manner as to be in the mixer that their aperture is also placed only a small piece above the granular mass.
Som tilførselsorganer for gas kan der anvendes gængse apparater, der er egnede til gastiHedning. Sidstnævnte an-35 ordnes på en sådan måde, at en gasstrøm af den til enhver tid ønskede temperatur, mængde og hastighed tilledes gennem blande-As gas supply means, conventional apparatus suitable for gas heating may be used. The latter is arranged in such a way that a gas stream of the desired temperature, quantity and velocity at all times is supplied through the mixing apparatus.
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apparatets chargeringsåbning.the charging port of the device.
På den side af blandeapparatet, hvor produktet fraføres, kan der på hensigtsmæssig måde være efterindskudt en frasugningskappe efter blandeapparatet, på undersiden af 5 hvilken kappe der kan være anbragt en opfangningsbeholder med et aftapningsorgan. Det er endvidere hensigtsmæssigt at rense den gasstrøm (afgangsgas), der kommer ud fra blandeapparatet, gennem et efterindskudt filter.On the side of the mixer where the product is dispensed, a suction cap may be post-inserted after the mixer, on the underside of which sheath may be provided a capture container with a draining means. Furthermore, it is appropriate to purify the gas stream (exhaust gas) coming out of the mixer through a post-injected filter.
Opbygning og arrangement af et apparat, der er særlig 10 eqnet til gennemførelse af den her omhandlede fremgangsmåde, er skematisk vist på tegningen. På denne har de angivne tal nedenstående betydning: 1 = blandeapparat, hvis omdrejningsretning kan vendes om 2 = tilgang for bærergranulat (kernemateriale) 15 3 = beholder med transportsnekke til omhylningsmateriale 4 = beholder med tilgang for bindemiddel 5 = spjæld til tilkobling af en luftvarmer 6 = luftvarmer 7 = opfangningsbeholder for færdigprodukt 20 8 = sigteorgan til fraskillelse af agglomerater 9 = luftfilter med ventilator 10 = cellesluse til aftapningsorganThe construction and arrangement of an apparatus particularly suitable for carrying out the method of the present invention is schematically shown in the drawing. On this, the figures given have the following meanings: 1 = mixer whose direction of rotation can be reversed 2 = access for carrier granules (core material) 3 3 = container with transport screw for wrapping material 4 = container with access for binder 5 = dampers for connection of an air heater 6 = air heater 7 = capture product for finished product 20 8 = screen means for separating agglomerates 9 = air filter with fan 10 = cell lock for drain means
Til yderligere belysning af den her omhandlede fremgangsmåde skal dennes gennemførelse i et apparatur af den på teg-25 ningen viste type beskrives som eksempel. De angivne tal henviser her i hvert tilfældetil tegningen. Det i begge sider åbne blandeapparat (1) fyldes først med bærergranulat (kernemateriale) via vippeorganet (2). Under blanding sker dernæst successivt eller eventuelt også samtidigt forstøvning af binde-30 midlet (vandige eller organiske opløsninger og emulsioner) via tilgangen (4) og tilledning af det findelte faststof, der anvendes som omhylningsmateriale, via transportsnekken (3). Tilsætningen af bindemiddel og omhylningsmateriale sker hurtigt. Der blandes dernæst indtil endt granulatdannelse. Blande-35 varigheden er i hvert tilfælde afhængig af arten og mængden af granulatet. I tilslutning dertil sker tørringen ved til-For further elucidation of the process of the present invention, its implementation in an apparatus of the type shown in the drawing is described by way of example. The figures given here refer in each case to the drawing. The mixer (1) open on both sides is first filled with carrier granules (core material) via the rocker (2). Then, during mixing, successive or possibly simultaneous atomization of the binder (aqueous or organic solutions and emulsions) is effected via the inlet (4) and feeding of the finely divided solid used as a coating material, via the transport screw (3). The addition of binder and wrapping material takes place quickly. The mixture is then mixed until granular formation is completed. The mixing duration is in each case dependent on the nature and amount of the granulate. In addition, the drying is done by adding
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ledning af en eventuelt af luftvarmeren (6) forvarmet gasstrøm via spjældet (5). Den minimalmængde gas, der transporteres gennem blandeapparatet, skal være så stor, at der ikke er nogen dampkondensering mulig. Det færdige granulat transporteres der-5 næst ved at vende blandeapparatets omdrejningsretning ind i opfangningsbeholderen (7) og føres via sigteorganet {8) til fraskillelse af eventuelt indeholdte agglomerater til aftapningsorganet (10). Afgangsgasserne suges gennem luftfilteret (9) ved hjælp af en ventilator.conduction of a gas stream possibly preheated by the air heater (6) via the damper (5). The minimum amount of gas transported through the mixer must be so large that no vapor condensation is possible. The finished granules are then transported by reversing the direction of rotation of the mixer into the capture container (7) and passed via the screening means (8) to separate any contained agglomerates to the draining means (10). The exhaust gases are sucked through the air filter (9) by means of a fan.
10 Ved en særlig udføreIsesform for den her omhandlede fremgangsmåde arbejder man således, at man til det færdige granulat yderligere sætter en coating-opløsning før tørringen.In a particular embodiment of the process of the present invention, one works in such a way that a coating solution is further added to the finished granules before drying.
Granulatpartiklerne forsynes derved med et yderligere omhyl- ningslag, hvorved den i forvejen høje modstandsevne mod af-15 gnidning hos de granulater, der kan fremstilles ifølge opfindelsen, forøges yderligere.The granulate particles are thereby provided with a further coating layer, thereby further increasing the already high resistance to rubbing of the granules which can be produced according to the invention.
De granulater, der kan fremstilles ved fremgangsmåden ifølge opfindelsen, er støvfrie og kan anvendes ved de inden for plantebeskyttelsen gængse fremgangsmåder.The granules which can be prepared by the process of the invention are dust-free and can be used in the methods of plant protection.
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Fremstillingen af støvfrie plantebeskyttelsesmiddel-' -granulater ved den her omhandlede fremgangsmåde illustreres ved hjælp af nedenstående eksempler.The preparation of dust-free plant protection granules by the process of this invention is illustrated by the following examples.
25 Sammenligningseksempel· 1.Comparative Example · 1.
Fremstilling af et granulat ved en fra teknikkens stade kendt fremgangsmåde: I et Nauta-blandeapparat anbringes først 460,0 kg kvartssand med kornstørrelsen 0,4 - 0,8 mm, og under blanding 30 tilsættes 5,0 kg hvid olie. Bærerstoffet er ensartet befug- tet efter ca. 5 minutter. Dernæst tilsættes 35,0 kg af en blanding af aktive forbindelser bestående af 40,0 vægtprocent 3-(3,4-dichlorphenyl)-l,l-dimethylurinstof, 20,0 vægtprocent 3-sek.butyl-5-brom-6-methyluracil, 28,5 vægtprocent 3-amino-35 -1,2,4-triazol og 11,5 vægtprocent kiselsyre. Efter ca.Preparation of a granulate by a method known in the art: In a Nauta mixer, first put 460.0 kg of quartz sand with the grain size of 0.4 - 0.8 mm and during mixing 30 5.0 kg of white oil is added. The carrier is uniformly wetted after approx. 5 minutes. Next, 35.0 kg of a mixture of active compounds consisting of 40.0% by weight of 3- (3,4-dichlorophenyl) -1,1-dimethylurea, 20.0% by weight 3-sec-butyl-5-bromo-6 is added. methyluracil, 28.5% by weight 3-amino-1, 1,2,4-triazole and 11.5% by weight silicic acid. After approx.
15-20 minutter er der dannet et ensartet omhylningslag på 1015-20 minutes, a uniform wrap layer of 10 is formed
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bærermaterialet. Hvis det fremkomne granulat stadig klæber, frembringes et fritstremmende produkt ved portionsvis tilsætning af meget findelt fyldstof (f.eks. kaolin).support material. If the resulting granule still adheres, a free-flowing product is produced by portionwise addition of very finely divided filler (e.g., kaolin).
5 Sammenliqningseksempel 2.Comparative Example 2.
Fremstilling af et granulat ved en fra teknikkens stade kendt fremgangsmåde: I et Munson-blandeapparat anbringes først 461,3 kg kvartssand med kornstørrelsen Q,4 - 0/8 mm, og dernæst til-10 sættes successivt 7,5 kg af en klæbemiddelopløsning (= 50%'s vandig polyvinylacetatemulsion) og 35,0 kg af en blanding af aktive forbindelser, der består af 40,0 vægtprocent 3-(3,4--dichlorphenyl)-l,l-dimethylurinstof, 20,0 vægtprocent 3-sek. butyl-5-brom-6-methyluracil, 28,5 vægtprocent 3-amino-l,2,4-15 -triazol og 11,5 vægtprocent kiselsyre. Efter ca. 5 minutter er der dannet et ensartet omhylningslag på bærermaterialet.Preparation of a granulate by a method known in the art: In a Munson mixer, 461.3 kg of quartz sand with the grain size Q, 4 - 0/8 mm is first placed, and then 7.5 kg of an adhesive solution is successively added ( = 50% aqueous polyvinyl acetate emulsion) and 35.0 kg of a mixture of active compounds consisting of 40.0% by weight of 3- (3,4-dichlorophenyl) -1,1-dimethylurea, 20.0% by weight of 3- SEC. butyl 5-bromo-6-methyluracil, 28.5% by weight 3-amino-1, 2,4-15-triazole and 11.5% by weight silica. After approx. 5 minutes, a uniform coating layer is formed on the support material.
Det fugtige granulat overføres til en modstrøms-drejerørs--tørrer.The moist granule is transferred to a countercurrent rotary tube dryer.
Lufttilgangstemperatur: 60 - 80°CAir supply temperature: 60 - 80 ° C
20 Tørringsvarighed: 10 - 15 minutter20 Drying Duration: 10 - 15 minutes
Restvandindhold i produktet: ^ 0,3%Residual water content of the product: ^ 0.3%
Produkttemperatur: ca. 40 - 50°CProduct temperature: approx. 40 - 50 ° C
Før aftapningen mellemlagres granulatet til afkøling.Before draining, the granulate is stored for cooling.
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Eksempel 1Example 1
Fremstilling af et granulat ved fremgangsmåden ifølge 30 opfindelsen: I et åbent blandeapparat af den på tegningen viste type anbringes først 461,3 kg kvartssand med kornstørrelsen 0,4 - 0,8 mm, og dernæst tilsættes successivt som bindemiddel 7,5 kg af en klæbemiddelopløsning (= 50%·s vandig polyvinyl-35 acetatemulsion) - blandetid 1 minut - og som plantebeskyttelsesmiddel og omhylningsmaterialer 35,0 kg af en blanding af aktive forbindelser, der består af 40,0 vægtprocent 3-(3,4- oPreparation of a granulate according to the method of the invention: In an open mixer of the type shown in the drawing, 461.3 kg of quartz sand with the grain size of 0.4 - 0.8 mm is first placed and then successively as a binder 7.5 kg of a adhesive solution (= 50% s aqueous polyvinyl-acetate emulsion) - mixing time 1 minute - and as a plant protection agent and wrapping materials 35.0 kg of a mixture of active compounds consisting of 40.0% by weight of 3- (3.4- o
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11 -dichlorphenyl)-l,1-dimethylurinstof, 20,0 vægtprocent 3--sek.butyl-5-brom-6-methyluraci1, 28,5 vægtprocent 3-amino-1, 2, 4-triazol og 11,5 vægtprocent kiselsyre. Efter ca. 5 minutter er der dannet et ensartet omhylningslag på bærer-5 materialet.11-dichlorophenyl) -1,1-dimethylurea, 20.0% by weight 3-sec-butyl-5-bromo-6-methyluracyl, 28.5% by weight 3-amino-1,2,4,4-triazole and 11,5% by weight silicic acid. After approx. 5 minutes, a uniform coating layer is formed on the support material.
Dernæst suges straks varmluft gennem blandeapparatet..Then hot air is immediately sucked through the mixer ..
Lufttilgangstemperatur: 50 - 70°CAir supply temperature: 50 - 70 ° C
Luftafgangstemperatur: 30 - 35°CAir outlet temperature: 30 - 35 ° C
Tørringsvarighed: 15-20 minutterDrying time: 15-20 minutes
Restvandindhold i produktet ^ 0,3%Residual water content of the product ^ 0.3%
Produktet har en temperatur på ca. 25°C og kan af- tappes uden efterindskudt afkølingsfase.The product has a temperature of approx. 25 ° C and can be drained without post-cooling cooling phase.
15 Bestemmelse af modstandsevnen mod afgnidning hos de ifølge sammenligningseksempel 1 og 2 samt eksempel 1 fremstillede granulater_ / 20 Som forsøgsapparatur anvendes et bægerglas med en indvendig diameter på 90 mm. I dette bægerglas fyldes i hvert tilfælde 100 g af det granulat, der skal afprøves. I en højde på 5 mm over bægerglassets bund drejer sig den vandrette bjælke (diameter 12 mm, længde 65 mm) i en T-formig omrører 25 med ca. 600 omdrejninger pr. minut. Efter 30 minutter frasigtes via en 200 pm forsøgssigte. Den fine andel, der passerer sigten, angives som % afgnidning.Determination of the abrasion resistance of the granules prepared according to Comparative Examples 1 and 2 and Example 1 As a test apparatus, a beaker with an internal diameter of 90 mm is used. In this beaker, in each case 100 g of the granulate to be tested is filled. At a height of 5 mm above the bottom of the beaker, the horizontal beam (diameter 12 mm, length 65 mm) rotates in a T-shaped stirrer 25 with approx. 600 rpm minute. After 30 minutes, a 200 µm test screen is discarded. The fine proportion passing the sieve is indicated as% abrasion.
Sammenlig- Sammenlig- ningseksempel 1 ningseksempel2 Eksempel 1 30 % afgnidning 3,5 1,5 0,5Comparative Comparative Example 1 Example 2 Example 1 30% trimming 3.5 1.5 0.5
Som det fremgår af de konstaterede procenttal, har det granulat, der er fremstillet ved den her omhandlede frem- qc gangsmåde (eksempel 1), en væsentlig højere modstandsevne modAs can be seen from the percentages found, the granulate produced by the method of the present invention (Example 1) has a significantly higher resistance to
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12 afgnidning end de granulater, der er fremstillede ved i forvejen kendte metoder (sammenligningseksempel 1 og 2) .12 than the granules prepared by methods known in the art (Comparative Examples 1 and 2).
Eksempel 2 5Example 2 5
Fremstilling af et granulat ved den her omhandlede fremgangsmåde : I et åbent blandeapparat af den på tegningen viste 10 type anbringes først 467,5 kg calcit med kornstørrelsen 0,5 - 1,0 mm. Dertil forstøves 15,0 kg klæbemiddelopløsning (20%'s vandig polyvinylalkoholopløsning) som bindemiddel under blanding. Efter 2 minutter tilsættes som plantebeskyttelsesmiddel og omhylningsmateriale 26,0 kg af en 2,2-dime-15 thyl-2,3-dihydrobenzofurany1-7-methy1carbamat-forb1ånding, der består af 75 vægtprocent 2,2-dimethyl-2,3-dihydroben-zofuranyl-7-methylcarbamat, 1,0 vægtprocent fugtemiddel, 5,0 vægtprocent dispergeringsmiddel, 0,8 vægtprocent hvid olie og 18,2 vægtprocent fyldstoffer, samt 0,7 kg jernoxid-20 rødt. Der blandes i 5 minutter. Dernæst suges varmluft gennem blandeapparatet.Preparation of a granulate by the process of the present invention: In an open mixer of the type shown in the drawing, 467.5 kg of calcite having a grain size of 0.5 - 1.0 mm are first placed. In addition, 15.0 kg of adhesive solution (20% aqueous polyvinyl alcohol solution) is atomized as a binder under mixing. After 2 minutes, 26.0 kg of a 2,2-dimethyl-2,3-dihydrobenzofuranyl-7-methylcarbamate compound consisting of 75% by weight 2,2-dimethyl-2,3- dihydrobenzofuranyl-7-methylcarbamate, 1.0 wt% wetting agent, 5.0 wt% dispersant, 0.8 wt% white oil and 18.2 wt% fillers, and 0.7 kg iron oxide-red. Mix for 5 minutes. Next, hot air is sucked through the mixer.
Lufttilgangstemperatur: 50 - 70°CAir supply temperature: 50 - 70 ° C
Luftafgangstemperatur: 30 - 35°CAir outlet temperature: 30 - 35 ° C
Tørringsvarighed: 30 - 35 minutterDrying duration: 30 - 35 minutes
Restvandindhold i produktet: £ 0,3%Residual water content of the product: £ 0.3%
Produkttemperatur: 25°CProduct temperature: 25 ° C
Det fremkomne granulat har en høj modstandsevne mod afgnidning.The resulting granulate has a high abrasion resistance.
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Fremstilling af et granulat ved den her omhandlede fremgangsmåde: 35 1 et åbent blandeapparat af den på tegningen viste type anbringes først 480,7 kg kvartssand med kornstørrelsenPreparation of a granulate by the process of the present invention: In an open mixer of the type shown in the drawing, 480.7 kg of quartz sand of the grain size is first placed
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13 0,4 - 0,8 ram. Dernæst tilsættes ved forstøvning som bindemiddel 15,0 kg af en klæbemiddelopløsning, der består af en 40%'s vandig polyvinylpyrrolidonopløsning. Derefter tilsættes som plantebeskyttelsesmiddel og omhylningsmateriale en homo-5 geniseret blanding af 8,3 kg 0-ethyl-0-(3-methyl-4-methyl-thio-phenyl)-isopropyl-amidophosphat, der består af 60 vægtprocent o-ethyl-O-(3-methyl-4-methylthio-phenyl)-isopropyl-amidophosphat og 40 vægtprocent kiselsyre, samt 5,0 kg lig-ninsulfonat (natriumsalt). Efter ca. 10 minutter er bærer-10 stoffet ensartet omhyllet, og tørringsprocessen begyndes.13 0.4 - 0.8 frame. Next, by spraying as a binder 15.0 kg of an adhesive solution consisting of a 40% aqueous polyvinylpyrrolidone solution is added. Then, as a plant protection agent and wrapping material, a homogenized mixture of 8.3 kg of 0-ethyl-O- (3-methyl-4-methyl-thio-phenyl) -isopropyl amidophosphate consisting of 60% by weight of o-ethyl O- (3-methyl-4-methylthio-phenyl) -isopropyl-amidophosphate and 40% by weight of silicic acid, as well as 5.0 kg of lignin sulfonate (sodium salt). After approx. For 10 minutes, the carrier-10 substance is uniformly wrapped and the drying process begins.
Lufttilgangstemperatur: 50 - 70°CAir supply temperature: 50 - 70 ° C
Luftafgangstemperatur: 30 - 35°CAir outlet temperature: 30 - 35 ° C
Tørringsvarighed: 20 - 25 minutterDrying time: 20 - 25 minutes
Restvandindhold i produktet: é* 0,5%Residual water content of the product: é * 0.5%
15 Produkttemperatur: 25°CProduct temperature: 25 ° C
Det fremkomne granulat har en høj modstandsevne mod afgnidning.The resulting granulate has a high abrasion resistance.
Eksempel 4 20Example 4 20
Fremstilling af et granulat ved den her omhandlede fremgangsmåde: I et åbent blandeapparat af den på tegningen viste type anbringes først 372,0 kg calcit med kornstørrelsen 0,5 25 - 1,0 mm, og under blanding tilsættes som bindemiddel 30,0 kg af en klæbemiddelopløsning (= 33%'s vandig stivelsesopløsning) og som plantebeskyttelsesmiddel og omhylningsmateriale 118,0 kg 2-isopropoxy-phenyl-N-methylcarbamat i form af et 70%'s befugteligt pulver (WP) bestående af 70% 2-isopropoxy-30 phenyl-N-methylcarbamat, 1,5% fugtemiddel, 6% dispergerings-middel og 7,5% fyldstof (f.eks. kaolin). Tilsætningen af disse komponenter er afsluttet efter 5-10 minutter. Derefter efterblandes der i 5 minutter for at gøre omhylningslaget fast. Derefter suges varm luft gennem blandeapparatet.Preparation of a granulate by the process of the present invention: In an open mixer of the type shown in the drawing, 372.0 kg of calcite of grain size of 0.5 25 - 1.0 mm is first applied, and while mixing 30.0 kg of binder are added as a binder. an adhesive solution (= 33% aqueous starch solution) and as a plant protection agent and coating material 118.0 kg of 2-isopropoxy-phenyl-N-methylcarbamate in the form of a 70% wettable powder (WP) consisting of 70% 2-isopropoxy 30 phenyl N-methylcarbamate, 1.5% wetting agent, 6% dispersant and 7.5% filler (eg kaolin). The addition of these components is completed after 5-10 minutes. Then mix for 5 minutes to secure the cover layer. Then hot air is sucked through the mixer.
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Lufttilgangstemperatur: 50°CAir supply temperature: 50 ° C
Luftafgangstemperatur: 30°CAir outlet temperature: 30 ° C
Tørringsvarighed: ca. 45 minutterDrying duration: approx. 45 minutes
Restvandindhold i produktet: £.1,0%Residual water content of the product: £ .1.0%
5 Produkttemperatur: ca. 20°C5 Product temperature: approx. 20 ° C
Det fremkomne granulat har en høj modstandsevne mod afgnidning.The resulting granulate has a high abrasion resistance.
Eksempel 5 10Example 5 10
Fremstilling af et granulat ved den her omhandlede fremgangsmåde ved imprægnering af et porøst bærerstof og påfølgende coating: 15 I et åbent blandeapparat af den på tegningen viste type anbringes først 173,0 kg pimpstengrus med kornstørrelsen 0,5-1,0 mm, og under blanding tilsættes som plantebeskyttelsesmiddel og bindemiddel en homogeniseret blanding af 4,0 kg emulgatoropløsning (= 80%'s opløsning af emulgatoren i 20 butanol) og 21,0 kg 2-(ethylthiomethyl-phenyl)-N-methylcarb-amat. Der efterblandes i 10 minutter til ensartet fordeling. Defter indsprøjtes som omhylningsmateriale 10,0 kg af en coating-opløsning (= 20%'s opløsning af polyvinylalkohol i vand). Derpå indledes tørringsprocessen straks: 25 oPreparation of a granulate by the process of this invention by impregnating a porous support and subsequent coating: In an open mixer of the type shown in the drawing, first 173.0 kg of pumice stone having a grain size of 0.5-1.0 mm is placed, and below mixture is added as a plant protection agent and binder a homogenized mixture of 4.0 kg of emulsifier solution (= 80% solution of the emulsifier in 20 butanol) and 21.0 kg of 2- (ethylthiomethyl-phenyl) -N-methylcarbamate. Mix for 10 minutes to evenly distribute. Defter is injected as a coating material with 10.0 kg of a coating solution (= 20% polyvinyl alcohol solution in water). Then the drying process begins immediately: 25 o
Lufttilgangstemperatur: 60 CAir supply temperature: 60 C
Luftafgangstemperatur: 30°CAir outlet temperature: 30 ° C
Tørringsvarighed: 10-15 minutterDrying duration: 10-15 minutes
Restvandindhold i produktet: £θ,3%Residual water content of the product: £ θ, 3%
Det fremkomne granulat har en høj modstandsevne mod 30 afgnidning.The resulting granulate has a high resistance to abrasion.
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Eksempel 6Example 6
Fremstilling af et granulat ved den her omhandlede fremgangsmåde ved imprægnering af et porøst bærerstof og 5 påfølgende coating: I et åbent blandeapparat af den på tegningen viste type anbringes først 167,4 kg pimpstengrus med kornstørrelsen 0,5 - 1,0 mm, og under blanding tilsættes som plantebeskyttelsesmiddel og bindemiddel en homogeniseret blanding af 10 10,8 kg 0,O-diethyl-S-(2-ethylmercaptoethyl)-dithiophosphor- syreester og 8,0 kg emulgatoropløsning (= 80%*s opløsning af emulgatoren i n-butanol). Dernæst påsprøjtes som omhyl-ningsmateriale en blanding af 15,0 kg urinstofopløsning (80%'s opløsning af urinstof i vand) og 16,5 kg formaldehyd-15 opløsning (40%'s opløsning af formaldehyd i vand). Den forløbende kondensation til urinstofharpiks accelereres ved tilsætning af 0,2 kg citronsyre. Samtidigt sker tørringen med en lufttilgangstemperatur på 60-70°C.Preparation of a granulate by the process of this invention by impregnating a porous support and subsequent coating: In an open mixer of the type shown in the drawing, first 167.4 kg of pumice stone having a grain size of 0.5 - 1.0 mm are placed, and below mixture is added as a plant protection agent and binder a homogenized mixture of 10.8 kg of O, diethyl-S- (2-ethylmercaptoethyl) -dithiophosphoric acid ester and 8.0 kg of emulsifier solution (= 80% * s solution of the emulsifier in n- butanol). Next, as a wrapping material, a mixture of 15.0 kg of urea solution (80% solution of urea in water) and 16.5 kg of formaldehyde solution (40% solution of formaldehyde in water) is sprayed. The progressive condensation for urea resin is accelerated by the addition of 0.2 kg of citric acid. At the same time, the drying takes place with an air inlet temperature of 60-70 ° C.
Luftafgangstemperatur: 30 - 35°CAir outlet temperature: 30 - 35 ° C
20 Tørringsvarighed: ca. 60 minutter20 Drying duration: approx. 60 minutes
Restvandindhold: 1,0 - 2,0%Residual water content: 1.0 - 2.0%
Det fremkomne granulat har en høj modstandsevne mod afgnidning.The resulting granulate has a high abrasion resistance.
25 30 3525 30 35
Claims (2)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19782804259 DE2804259A1 (en) | 1978-02-01 | 1978-02-01 | METHOD FOR PRODUCING DUST-FREE PLANT PROTECTION AGENT GRANULES AND DEVICE FOR CARRYING OUT THE METHOD |
| DE2804259 | 1978-02-01 |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| DK40679A DK40679A (en) | 1979-08-02 |
| DK155771B true DK155771B (en) | 1989-05-16 |
| DK155771C DK155771C (en) | 1989-10-09 |
Family
ID=6030900
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DK040679A DK155771C (en) | 1978-02-01 | 1979-01-31 | PROCEDURE FOR THE PREPARATION OF DUST-FREE PLANT PROTECTIVE GRANULATES |
Country Status (18)
| Country | Link |
|---|---|
| EP (1) | EP0003302B1 (en) |
| JP (1) | JPS54110979A (en) |
| AR (1) | AR222987A1 (en) |
| AT (1) | AT367266B (en) |
| AU (1) | AU526241B2 (en) |
| BR (1) | BR7900597A (en) |
| CA (1) | CA1122897A (en) |
| DE (2) | DE2804259A1 (en) |
| DK (1) | DK155771C (en) |
| ES (1) | ES477316A1 (en) |
| IL (1) | IL56527A (en) |
| KE (1) | KE3246A (en) |
| NZ (1) | NZ189493A (en) |
| OA (1) | OA06170A (en) |
| PH (1) | PH17481A (en) |
| PT (1) | PT69134A (en) |
| TR (1) | TR20872A (en) |
| ZA (1) | ZA79403B (en) |
Families Citing this family (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0027989A1 (en) * | 1979-10-24 | 1981-05-06 | Bernard Dr. Delley | A process for preparing a rodenticidal bait |
| EP0107107B1 (en) * | 1982-10-04 | 1987-01-14 | O.M.Scott + Sons Company | Granulated plant protection agent and process for its preparation |
| DE3300374A1 (en) * | 1983-01-07 | 1984-07-12 | Bayer Ag, 5090 Leverkusen | METHOD FOR DEDUSTING AN ABRASION-SENSITIVE PRODUCT |
| US7241500B2 (en) | 2003-10-06 | 2007-07-10 | Certainteed Corporation | Colored roofing granules with increased solar heat reflectance, solar heat-reflective shingles, and process for producing same |
| FR2884111B1 (en) * | 2005-04-07 | 2007-05-18 | Saint Gobain Mat Constr Sas | BIOCIDAL GRANULE, IN PARTICULAR FOR THE MANUFACTURE OF ASPHALT SHINGLE |
| US9044921B2 (en) | 2005-09-07 | 2015-06-02 | Certainteed Corporation | Solar heat reflective roofing membrane and process for making the same |
| US7749593B2 (en) | 2006-07-07 | 2010-07-06 | Certainteed Corporation | Solar heat responsive exterior surface covering |
| CA2688340C (en) | 2007-05-24 | 2016-02-09 | Certainteed Corporation | Roofing granules with high solar reflectance, roofing products with high solar reflectance, and processes for preparing same |
| WO2009145968A1 (en) | 2008-03-31 | 2009-12-03 | Certainteed Corporation | Coating compositions for roofing granules, dark colored roofing granules with increased solar heat reflectance, solar heat-reflective shingles, and process for producing the same |
| US8394498B2 (en) | 2008-12-16 | 2013-03-12 | Certainteed Corporation | Roofing granules with high solar reflectance, roofing materials with high solar reflectance, and the process of making the same |
| US8637116B2 (en) | 2009-08-20 | 2014-01-28 | Certainteed Corporation | Process for preparing roofing granules comprising organic colorant, with improved luster, and roofing products including such granules |
| US8722140B2 (en) | 2009-09-22 | 2014-05-13 | Certainteed Corporation | Solar heat-reflective roofing granules, solar heat-reflective shingles, and process for producing the same |
| US9540822B2 (en) | 2009-11-24 | 2017-01-10 | Certainteed Corporation | Composite nanoparticles for roofing granules, roofing shingles containing such granules, and process for producing same |
| US20110223385A1 (en) | 2010-03-15 | 2011-09-15 | Ming Liang Shiao | Roofing granules with high solar reflectance, roofing products with high solar reflectance, and process for preparing same |
| CA2783777A1 (en) | 2011-08-18 | 2013-02-18 | Certainteed Corporation | System, method and apparatus for increasing average reflectance of a roofing product for sloped roof |
| US10730799B2 (en) | 2016-12-31 | 2020-08-04 | Certainteed Corporation | Solar reflective composite granules and method of making solar reflective composite granules |
| WO2023156946A1 (en) * | 2022-02-17 | 2023-08-24 | Pi Industries Ltd. | Dust-free granules and method for producing same |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2100849A1 (en) * | 1970-07-01 | 1972-03-24 | Fisons Ltd | |
| GB1299378A (en) * | 1969-12-05 | 1972-12-13 | Fruitgrowers Chemical Company | Granules for the application of agricultural chemicals |
| GB1304543A (en) * | 1969-03-15 | 1973-01-24 | ||
| GB1305320A (en) * | 1970-07-23 | 1973-01-31 | ||
| FR2289252A1 (en) * | 1974-11-01 | 1976-05-28 | Fisons Ltd | Absorbent substrate esp peat coated with fine powder - and finally with adhesive liq giving firm bonding of powder to substrate (NL040576) |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB622374A (en) * | 1946-03-16 | 1949-05-02 | Du Pont | Improvements in and relating to the photo-polymerisation of compounds containing theethylene double bond |
| DE1720367A1 (en) * | 1966-03-08 | 1971-07-08 | Ceskoslovenska Akademie Ved | Process for the production of polymers by photoinitiation and suitable initiators |
| DE2130070C3 (en) * | 1971-06-18 | 1981-08-20 | Röhm GmbH, 6100 Darmstadt | Process for the photopolymerization of acrylic, methacrylic compounds or styrene in the presence of azo compounds |
| JPS52117292A (en) * | 1976-03-30 | 1977-10-01 | Takeda Chem Ind Ltd | Production of granular catalyst or catalyst carrier |
-
1978
- 1978-02-01 DE DE19782804259 patent/DE2804259A1/en not_active Withdrawn
-
1979
- 1979-01-15 DE DE7979100103T patent/DE2960447D1/en not_active Expired
- 1979-01-15 EP EP79100103A patent/EP0003302B1/en not_active Expired
- 1979-01-26 PT PT7969134A patent/PT69134A/en unknown
- 1979-01-29 NZ NZ189493A patent/NZ189493A/en unknown
- 1979-01-29 IL IL56527A patent/IL56527A/en unknown
- 1979-01-30 PH PH22141A patent/PH17481A/en unknown
- 1979-01-30 JP JP882379A patent/JPS54110979A/en active Pending
- 1979-01-30 TR TR20872A patent/TR20872A/en unknown
- 1979-01-30 AT AT0067479A patent/AT367266B/en not_active IP Right Cessation
- 1979-01-31 CA CA320,614A patent/CA1122897A/en not_active Expired
- 1979-01-31 AR AR275356A patent/AR222987A1/en active
- 1979-01-31 ES ES477316A patent/ES477316A1/en not_active Expired
- 1979-01-31 ZA ZA79403A patent/ZA79403B/en unknown
- 1979-01-31 DK DK040679A patent/DK155771C/en not_active IP Right Cessation
- 1979-01-31 BR BR7900597A patent/BR7900597A/en unknown
- 1979-02-01 OA OA56723A patent/OA06170A/en unknown
- 1979-02-01 AU AU43854/79A patent/AU526241B2/en not_active Ceased
-
1982
- 1982-11-26 KE KE3246A patent/KE3246A/en unknown
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1304543A (en) * | 1969-03-15 | 1973-01-24 | ||
| GB1299378A (en) * | 1969-12-05 | 1972-12-13 | Fruitgrowers Chemical Company | Granules for the application of agricultural chemicals |
| FR2100849A1 (en) * | 1970-07-01 | 1972-03-24 | Fisons Ltd | |
| GB1305320A (en) * | 1970-07-23 | 1973-01-31 | ||
| FR2289252A1 (en) * | 1974-11-01 | 1976-05-28 | Fisons Ltd | Absorbent substrate esp peat coated with fine powder - and finally with adhesive liq giving firm bonding of powder to substrate (NL040576) |
Also Published As
| Publication number | Publication date |
|---|---|
| BR7900597A (en) | 1979-08-28 |
| PH17481A (en) | 1984-09-03 |
| DK155771C (en) | 1989-10-09 |
| CA1122897A (en) | 1982-05-04 |
| PT69134A (en) | 1979-02-01 |
| ES477316A1 (en) | 1979-07-01 |
| EP0003302B1 (en) | 1981-07-08 |
| JPS54110979A (en) | 1979-08-30 |
| IL56527A0 (en) | 1979-03-12 |
| EP0003302A1 (en) | 1979-08-08 |
| OA06170A (en) | 1981-06-30 |
| KE3246A (en) | 1983-01-28 |
| NZ189493A (en) | 1980-08-26 |
| AR222987A1 (en) | 1981-07-15 |
| AU526241B2 (en) | 1982-12-23 |
| TR20872A (en) | 1982-11-18 |
| ZA79403B (en) | 1980-02-27 |
| IL56527A (en) | 1982-09-30 |
| ATA67479A (en) | 1981-11-15 |
| AT367266B (en) | 1982-06-25 |
| DK40679A (en) | 1979-08-02 |
| AU4385479A (en) | 1979-08-09 |
| DE2804259A1 (en) | 1979-08-02 |
| DE2960447D1 (en) | 1981-10-15 |
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| Date | Code | Title | Description |
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| PBP | Patent lapsed |