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NZ203127A - Water-dispersible or water-soluble granules their production and use - Google Patents

Water-dispersible or water-soluble granules their production and use

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Publication number
NZ203127A
NZ203127A NZ203127A NZ20312783A NZ203127A NZ 203127 A NZ203127 A NZ 203127A NZ 203127 A NZ203127 A NZ 203127A NZ 20312783 A NZ20312783 A NZ 20312783A NZ 203127 A NZ203127 A NZ 203127A
Authority
NZ
New Zealand
Prior art keywords
weight
parts
water
granules
granules according
Prior art date
Application number
NZ203127A
Inventor
H Hausmann
H Neumaier
Original Assignee
Bayer Ag
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bayer Ag filed Critical Bayer Ag
Publication of NZ203127A publication Critical patent/NZ203127A/en

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Classifications

    • 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
    • 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
    • A01N25/14—Powders or granules wettable
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/0002—Galenical forms characterised by the drug release technique; Application systems commanded by energy
    • A61K9/0007—Effervescent

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Public Health (AREA)
  • Agronomy & Crop Science (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Animal Behavior & Ethology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Medicinal Chemistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Toxicology (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Glanulating (AREA)

Description

New Zealand Paient Spedficaiion for Paient Number £031 £7 2 031 2 7 <fE?- ? i* h Priority Date(s): (^Iplete Specification Filed: 2X-. lr£3 Cass: A*Wax/A* ^iXi/c© Publication Date: 3.0. .. 737ft.
P.^RJourna!, No: KIRW ZEALAND Patents Act. 1953 W N.Z. NO. • CV COMPLETE SPECIFICATION "Water-dispersible or water-soluble granules, a process for their'production, and their use." We, BAYER AKTIENGESELLSCHAFT, a Company registered under the laws of the Federal Republic of Germany, of Leverkusen, Germany, do hereby declare the invention, for which we pray that a Patent may be granted to us, and the method by which it is to be performed, to be particularly described in and by the following statement (Followed by 1A.) - lfl- 203127 Type. V ; The present invention relates to new water-dispersible or water-soluble granules, to a process for their production, and to their use.
It has already been disclosed that water-5 dispersible granules are f ormed by a mixing and rolling motion of the material to be granulated, in appropriate apparatuses, with si muItaneous addition of smaI I amoun t s of I iquid (water or water and organic solvents) (see ' H.S. Ries "AufbaugranuI i erung (Layering granulation) in 10 Aufbereitungstechnik 11 (1971), pages 675 et seq.).
Furthermore, it is already known that water-dispersible granules may be produced by adding, to the material to be granulated, in a granulation drum, an amoun t of granulating liquid such that the equilibri um 15 moisture content of this material is exceeded, and then drying the resulting product again until the mo i s t u re con t en t reaches the equi I ibrium mo isture content or falls b e I ow this.
In addition, the production of water-dispersibIe granules by the fluidised bed process has already been described (see U.S. Patent Specification 3,920,442). In this process, the finely divided material is sprayed with an aqueous solution which contains a binder. 25 Finally, it isalso kn own that wa ter-di spersible or water-soluble granules may be produced by the spray-drying process and by tabletting powder mixtures or by moulding powder mixtures. that in general a relatively high mechanical effort is required, and the processes are difficult to control, since many parameters have to be taken into account during The disadvantages of these known processes are the production. In addition, these granules in many cases are loose materials which have a low bulk density bit A 2'1 k3% 203127 and which therefore possess a relatively large packing volume. Moreover, granules of this type tend to form dust, and are not always easy to disperse or dissolve in an aqueous medium, since their density is lower than that of water. A further disadvantage is that the granules produced by these known processes frequently have very variable particle size, that is to say they possess a broad particle size spectrum. The dispersibility or solubility, in water, of the granules or pellets obtainable by the kncwn moulding or tabletting processes is also not always satisfactory.
The present invention now provides a water-dispersible or water-soluble granules which contain (1) 5 to 80% by weight of at least one active component, (2) 5 to 30% by weight of at least one product capable of producing gas, (3) 2 to 60% by weight of one or more additives and, if necessary, (4) 1 to 20% by weight of granulating liquid, the sum of the constituents being 100% by weight in each case.
The present invention further provides a process for the productien of water-dispersible or water-soluble granules according to the invention in which (a) at least one active component (1) is mixed with at least cne product (2) capable of producing gas, and with additive(s) (3), (b) the resulting mixture is finely milled, thereafter granulating liquid (4) is added, and the mixture is dried if desired and (c) the mixture is pelleted or tabletted, the constituents being added in amounts, such.that the granules contain i weight of constituent to 80% by weight of constituent (1)f 5 to . 30% by|(2), 2 to 60% by weight of additive(s) (3) and 1 to 20% by weight of granulating liquid (4), with the sum of the constituents being 100% by weight in each case, and the active component, if liquid at roan temperature having been absorbed, before granulation, on a solid carrier.
Finally, it has been found that the water-dispersible or water-soluble granules according to the invention, depending on the active components present, can be used for the most diverse purposes in agriculture and in horticulture, in the household field and hygiene field, in the medical field or in the dyestuff industry.
A It is to be regarded as extremely surprising that n rt ml? 203127 the granules according to the invention are completely and rapidly dispersible or soluble in water, since, with the relatively high density and compactness of the agglomerates according to the invention, sedimentation and the 5 formation of lumps in water were to have been expected i n s t ead.
The water-dispersibIe or water-soluble granules according to the invention are distinguished by a number of advantages. Thus, these granules possess a high den-10 sity and a high bulk density, as a result of which the pack i ng volume i s smaII. It is also advantageous that these mechanically tabletted or pelleted granules have a variable particle size which is uniform within narrow limits, and me tering is therefore without problems. Fu r-15 thermore, owing to their mechanical strength, the granules according to the invention produce little dust, and are also resistant to abrasion in the case of all mechan i caI loads occurring in practice. The process, according to the invention, for the production of water-di spersib I e 20 or wa ter-soluble granules requires little expense in respect of machines and personnel, and is simple to monitor. In addition, the consumption of energy is comparatively low, since the drying process is superfluous in many cases. Moreover, the process according to the invention 25 is not limited to the granulation of a f ew substances, but is ex t remely widely applicable in respect of the active components. Finally, it can be carried out both continuously and discontinuousIy, regardless of the amount of material to be granulated, and permits a rapid change 30 of product, without complications.
The granules according to the invention can contain one or even several active components. Suitable active components are both those substances which are solid at r oom t emp erature and those wh ich are liquid at 35 room t emp erature. A precondition for using liquid active components is only that they be absorbed, before granulation, on solid carriers. The active c omp on en t s may be soluble or insoluble in water.
Suitable active components are agrochemical substances, active compounds for combating pests in the 5 household field and hygiene field, pharmacologically active substances and dyestuffs.
In this context, agrochemical substances are understood as meaning active compounds which can customarily be used in plant protection. These preferably 10 include insecticides, acaricides, nematicides, fungicides, herbicides, g rowt h regulators and fertilisers. The foilow-i ng may b e men tioned individually as examples of active compounds of this type: 0,0-diethyl 0-(4-nitro-phenyl) thiono-phosphate, 0,0-di me thyl 0-(4-ni tro-phenyl ) thiono-15 phosphate, 0 — e t hyI-0-(4-me thylthio —phenyl) S-propyl di thiophosphate, (0,0-di ethyl thionophosphoryl )-«(-oximino-phenylacetic acid nitrile, 2-isopropoxy-phenyl.N-methyl — ca rbama t e, 3-me thyl t h i o-4-ami no-6-tert .-butyl-1,2,4-tri-azin-5-one, 3-me thyl thio-4-isobutyl ideneamino-6-tert .-20 butyI - 1,2,4-triazin-5-one, 2-chIoro-4-ethyI ami no-6-i so-propylamino-1,3,5-triazine, 2,3-dihydro-2,2-di me thy I-7-benzofuranyl methyI-carbamate, 3,5-dimethyI-4-methyI -thiophenyl N-methyI-carbamate, 0,0-dietnyl 0-(3-chloro-4-methyI-7-coumarinyI ) thiophosphate, u-hexachIorocyclo-25 hexane, 6,7,8,9, 10, 10-hexachIoro-1 ,5 , 5A , 6 , 9,9A-hexahydro- 6,9-me thane-2,4,3-benzo-di oxa thiepin-3-oxide, 1,4,5,6,7,8,8-heptachloro-4,7-endo-me thy Iene-3A,4,7,7A-tet rahydroi ndene, 2-(fur-2-yl )-benzimidazole, 5-amino-1-bis-(di me thylami do)-.phosphoryl-3-phenyl-1, 2,4-triazole, 4-hydr oxy -3— (1,2,3,4-30 tetrahydro-naphth- 1-yI )-coumarin, S-£l ,2-bis-(ethoxy-carbonyl)-ethyl^J 0,0-di me thyl dithiophosphate, 0,0-di-methyl 0-(4-methyI mereapto-3-methyI-phenyI ) th i onophos-phate, 0-ethyl 0-(2-i sopropoxycarbonyI-phenyI ) N-iso-propyI-thionophosphori c acid ester amide, 1-(4-chloro-35 ph en oxy)-3,3-d i me thyl-1-(1.2,4-triazol-1-yl )-butan-2-one, (S)-o(-cyano-3-phenoxybenzy I ( 1 R ) - c i s-3 - ( 2 , 2-d i b romov i ny I ) - 203127 2,2-dimethylcycl.opropanecarboxylate.
Active compounds for combating pests in the household field and hygiene field are to be understood as meaning, in the present case substances which can be customarily 5 employed for purposes of this type. The following may be mentioned as examples: 2-isopropoxyphenyl N-methyl-carbamate, 0,0-diethyl 0-(4—nitro-phenyl) thionophos-phate, 0,0-dimethyl 0-(4-nitro-phenyl) thionophosphate, S-[1,2-bis-(ethoxycarbonyl)-ethyl] 0,0-dimethyl 10 dithiophosphate, 0,0-dimethyl 0-(3-methyl-4-nitrophenyl) thionophosphate, 0,0-dimethyl 0-(4-methylmercapto-3-methyl-phenyl) thionophosphate and cyclohex-l-ene—1,2-dicarboximidomethyl 2,2-dimethyl-3-(2-methylpropenyl)-cyclo-propanecarboxylate.
Pharmacologically active substances are to be understood as meaning, in the present case, substances which are preferably employed in the field of veterinary medicine. The following may be mentioned as an example of active compounds of this type: -cyano-3-phenoxy-4-20 fluoro-benzyl 2, 2-dimethyl-3-[ (1 - (p-chlorophenyl) - @ -chloro-vinyl]-cyclopropanecarboxylate.
Dyestuffs, as active component(s), are to be understood as meaning, in the present case, substances which are suitable for the preparation of dyestuff dispersions or dye-25 stuff solutions, which are used as colorants and/or paints. The following may be mentioned as examples: triarylamine dyestuffs:, triarylmethane dyestuffs, methine dyestuffs, anthraquinone dyestuffs, indigo dyestuffs, sulphur dyestuffs, azo dyestuffs and pigment dyestuffs. 30 The granules according to the invention can contain, as products capable of producing gas, any of those substances or substance mixtures which are capable of releasing gas when the granules are dispersed or dissolved in water, and which do not react with the particular 35 active components present. Gas producers of this type preferably include products which, under the stated 2031 2 conditions, can function as carbon dioxide donors or nitrogen donors, such as, for example, mixtures of an acid and a carbonate, mixtures of an acid anhydride and a carbonate, substances wh ich split off nitrogen, and mi x-5 tures which consist of bacteria and lactic acid and are capable of producing carbon dioxide.
The foilow i ng may b e men tioned as acids wh i ch can be present in the mixtures comprising an acid and a carbonate: saturated or unsaturated aliphatic mono-, di-10 and tricarb oxylie acids and hyd roxy carboxylic acids, such as acetic acid, propionic acid, succinic acid, adipic acid, citric acid, propanetricarboxylic acid, ma Ie i c acid, fumaric acid and aconitic acid, and also aminoacids, such as glycine, and furthermore optionally substituted mono-15 sulphonic acids, such as di-isobutyInaphtha I enesuIphonic acid and n-dodecyIbenzenesuIphon i c acid, and also optionally substituted a roma tic carboxylic acids, such as benzoic acid, terephthalic acid, bile acids and resin acid, and finally carboxylic acids derived f rom heterocycl ic 20 structures, such as nucleic acids.
The foilow i ng may be mentioned as ca rboxylie acid anhydrides which may be present in the mixtures comprising an acid anhydride and a carbonate: ma Ieic acid anhydride and phthalic acid anhydride.
Suitable carbonates which may be present in the mixtures comprising an acid or acid anhydride and a carbonate are natural and synthetic carbonates and bicarbon-ates. The foilow i ng may b e men t i on ed sp ec i f i caI Iy: alkali metal and alkaline earth metal carbonates or bicar-30 bonates, such as sodium bicarbonate, potassium carbonate, calcium carbonate, calcite, aragonite, li me stone, chalk, marble, magnesium carbonate, magnesium sulphate, calc-spar, calcium ca rb ona t e/magn e s i um carbonate mixture, pearl spar, d o I om ite, be ry I Mum carbonate and strontium carbon-35 ate, and also i ron(II) carbonate, iron spar, siderite, manganese carbonate, rhodochrosite, zinc spar, zinc 203127 carbonate and calamine.
The foilow i ng may be mentioned as exampIes of p roduc t s wh ich are capable of splittingoff nitrogen: diazonium salts, such as, for example, benzenediazonium g chI or i de.
Suitable additives wh i ch may be present in the granules according to the invention are surface-active substances, dispersing agents, extenders, binders, preservatives and dyestuffs.
For this purpose, preferred surface-active sub stances are surface-active substances of an anionic, cationic or non-ionic nature, as described, for example, in "T ensi de-T ext i Ihi If smi t t eI-Wa schrohstoffe (Surfactants -Textile Auxiliaries - Detergent Base Ma terials)" volume 1 , 15 pages 571 - 835, 837 - 917 and 963 - 1041 (1964), and in "GrenzfIMchenakt ive EthyI en oxid-Addukte (Surface-Active Ethylene Oxide Adducts)", pages 42 - 95 (1976). The foilow i ng may b e men tioned specifically: lignin suIph on -ate, methyIceI IuIose, poIyoxyethyI ene fatty acid esters, 20 poIyoxyethyI ene fatty alcohol ethers, for example a I ky I-aryI polyglycol ethers, alkyl sulphonates and albumin hydroIysation products.
Preferred dispersing agents are: condensation products of aromatic sulphonic acids and formaldehyde, 25 such as condensation products of sulphonated ditolyl ether and formaldehyde, and also I igninsuIphonic acid salts, such as lithi um saI t s, sod i um salts, potassi um salts, magnesium salts, calcium salts and ammonium salts of ligninsulphonic acid.
Suitable extenders are all fillers and carriers wh ich can cust oma rily be used in wa ter-dispersible or water-soluble granules. Substances of this type which can be pref erably used are inorganic salts, such as alkali metal, magnesium and ammonium chlorides and sulphates, 35 for example magnesium sulphate, potassium sulphate, sodium sulphate, potassium chloride, ammonium sulphate, lithium sulphate and ammon ium chloride, silicates, such as talc, chalk, quart z meal , kaolin, mon t mor illonite, b en -tonite and sepiolite, as well as graphite, and urea and urea derivatives, such as hexamethyI enetetramine and 5 casein, and furthermore carbohydrates, such as starch, sugar, alginates and their derivatives, cereal meals, such as wheat meal and rice meal, and also Kelzans, methyIceI IuIose and hydroxypropy I-methyIce1 IuIose, and finally water-soluble polymers, such as polyvinyl alcohol 10 and poIyvinyIpyrroI idone.
All binders (adhesives) wh i ch are cu s t oma ri Iy present in water-dispersibIe or water-soluble granules may be present as binders. These preferably include methyl-cellulose, sugar, dextrin, starch, alginates, glycols, 15 po I y v i ny I py r ro I i done , li gn i n sulphonate, gum arabic, polyvinyl alcohol and polyvinyl acetate.
Examples of preservatives which may be present in the granules according to the invention are 2-hydroxy-biphenyl, sorbic acid, p-hydroxybenzaldehyde, methyl 20 p-hydroxybenzoate, benzaIdehyde, benzoic acid and propyl p-hy d r oxy b en zoa t e .. Inorganic pigments, such as iron oxide, titanium dioxide and Prussian Blue, and organic dyestuffs, such as alizarin dyestuffs, azo dyestuffs and metal phtha Iocyanine dyestuffs, may be mentioned as dye-25 stuffs which are suitable additives.
The granules according to the invention can contain, as granulating liquids, wa ter, organic solvents or mixtures of water and organic solvents. Preferred organic solvents for this purpose are alcohols, such as ethanol 30 and glycol, ha Iogenohydrocarbons, such as methylene chloride, and ethers, such as dioxane and tetrahydrofuran.
Wa ter is a particularly preferred granulating liquid.
In the granules according to the invention, the proportions, in per cent, of the components present can 3 5 be varied within the stated relatively wide ranges. The proportion of active component or of active components (1) is 203127 between 5 and 80% by weight, preferably between 10 and 70% by weight. The proportion of the material capable of producing gas (2) is 5 to 30% by weight, preferably 10 to 28% by weight. The additives (3) are present in propor^ 5 tions between 2 and 60% by weight, preferably between 5 and 50% by weight, and the proportion of granulating liquid (4) is between 1 and 20% by weight, preferably between 3 ■ and 8% by weight.
In the production of the granules according to the 10 invention, it is preferable to select the components from all of those which have already been mentioned as being preferred in connection with the foregoing description of the granules according to the invention.
If, in the process according to the invention, one or 15 more active components which are liquid at room temperature are used, it is necessary to absorb these components, before granulation, on solid carriers.
In the process according to the invention, the process temperatures can be varied within a relatively wide range. 20 In general, the process is carried out at temperatures between 10 and 80°C, preferably between 20 and 60°C.
The process according to the invention is carried out in general under atmospheric pressure. However, it is also possible to employ elevated or reduced pressure. 25 In carrying out the process according to the invention, the following procedure is in general followed: first, at least one active component is mixed, in the desired weight ratio, with at least one product capable of producing gas, and with additives, this pulverulent 30 mixture is finely milled, and thereafter granulated in a mixer, by adding 1 to 20% by weight, preferably 2 to 10% by weight, relative to the resulting product, of granulating liquid, this product is dried if desired and then pelleted or tabletted.
The process according to the invention can be M"»im carried out both continuously and di scont inuousIy .
To carry out the mi I I ing process, customary dry-comminuting apparatuses are used in the process according to the invention. Preferred mills are ball mills, rotor/ 5 stator mills, pinned disc mills, hammer mills and jet mills, if appropriate with suitable downstream separators.
The treatment of the pulverulent material with the granulating liquid can be carried out in any of the customary mixing apparatuses. Any of the driers which are customarily 10 used in the production of granules are suitable for drying, which is not absolutely necessary. The final actual production of the granules is effected in customary tabletting or pelleting presses.
In the process according to the invention, the 15 granules obtained are c ompa c t, produce little dust, have a high density, and are of substantially unif orm shape and size. C ompa red with conventionally produced granules, the granules according to the invention are distinguished by i mp roved dispersibility or solubility in wa ter. 20 Depending on the active components present, the granules according to the invention can be employed for the most diverse purposes. Those granules which contain agrochemical active compounds as active components can be used according to customary methods in plant protection. 25 For example, granules of this type are dispersed or dissolved in water. The resulting dispersions or solutions, if appropriate after prior dilution, can be applied to the plants and/or their habitat according to customary methods, that is to say, for example, by injecting, spray-30 ing or pouring. In this case, the amount used depends on the concentration of thedi spersi on or solution, on the particular indication and on the active components present.
If the granules according to the invention contain 35 no agrochemical active compounds, but other active components, they are used according to methods which are T® V. ; 9 - 1 1 - customary in the particular area of industry. In this case, also, the amount used depends on the particular active components and the particular indication.
The production of the granules according to the 5 invention, and their i mp roved wa ter-di spersibi I i ty in com-parison with previously known granules, can be seen from the examples which follow.
Preparative examples Comparative Example A 10 70 parts by weight of 4-amino-3-methyI-6-phenyI - 1 , 2 , 4-t r i a z i n-5 ( 4H )-on e aremixed intensivelywith 4 parts by weight of alkylaryl sutphonate, 6 parts by weight of kaolin and 10 parts by weight of sulphite wa s t e liquor, and the mixture is milled in a mechanical mill. After 15 6 parts by weight of water have been added and thorough mixing has be en effect ed, the pre-fnix ' s converted to layered granules in a pelletising ma ch i n e. AggIomera t es which do not disperse readily in water are obtained in this mann e r.
Examples according to the invention ExampIe 1 70 parts by weight of 4-amino-3-methyI-6-phenyI -1,2,4-triazin-5(4H)-one are mixed intensively with 4 parts by weight of alkylaryl su I ph.ona:t e, 6 parts by weight of 25 kaolin, 5 parts by weight of adipic acid, 5 parts by weight of sodium bicarbonate and 10 parts by weight of sulphitewaste liquor, and the mixture is milled in a mechan ical mill. After 6 parts by weight of wa ter have been added and thorough mixing has been effected, the 30 pre-mix is converted to layered granules in a pelletising machine. A dust-free and free-flowing product which is readily dispersible in wa ter is obtained in this mann er. ExampIe 2 70 parts by weight of 4-amino-3-methyI-6-phenyI -35 1,2,4-triazin-5(4H)-one are mixed intensively with 5 parts by weight of adipic -acid, 5 parts by weight of sodium - 1 2 - bicarbonate and 20 parts by weight of sulphite waste liquor, and the mixture is milled in a jet mill. After 7 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to 5 layered granules in a pelletising mach ine, the particles having a diameter of 2 mm and a length of 3 mm. A product wh ich is readily dispersible in wa ter is obtained in this manner. The resulting dispersion may be satisfactorily applied, without difficulty, using a syringe. ] 0 ExampIe 3 70 parts by weight of 4-amino-3-methyI-6-phenyI -1,2,4-triazin-5(4H)-one are mixed intensively with 5 parts by weight of citric acid, 5 parts by weight of dolomite and 20 parts by weight of sulphite waste liquor, and the 15 mixture is milled in a mechanical mill. After 6 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising machine. A dust-free and f ree-fIow ing product wh ich is readily dispersible in wa ter 20 's obtained in this manner.
ExampIe 4 70 parts by weight of 4-amino-3-methyI-6-phenyI -1,2,4-triazin-5(4H)-one are mixed intensively with 5 parts by weight of citric acid, 5 parts by weight of dolomite 25 and 20 parts by weight of a IkyIaryI sulphonat e, and the mixture is milled in a mechanical mill. After 6 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising machine. A dust-free and 30 free-flowing product which is readily dispersible in water is obtained in this manner.
ExampIe 5 70 parts by weight of 4-amino-6-tert.-butyI-3-methyIthio-1,2,4-triazin-5(4H)-one are mixed intensively 35 with 6 parts by weight of kaolin, 5 parts by weight of adipic acid, 5 parts by weight of sodium bicarbonate and - 1 3 - 14 parts by weight of diphenyl ether-suIphonic acid-formaldehyde condensate, and the mixture is milled in a mech-anical mill. After 8 parts by weight of wa ter have been added and thorough mixing has been effected, the pre-mix 5 is converted to layered granules in a pelletising ma ch i n e. A dust-free and free-flow ing product wh i ch is read i Iy dispersible in water is obtained in this manner.
ExampIe 6 70 parts by weight of 4-amino-6-1ert.-butyI-3-10 methyIthio-1,2,4-triazin-5(4H)-one are mixed intensively with 10 parts by weight of adipic acid, 5 parts by weight of magnesium carbonate and 15 parts by weight of diphenyl ether-suIphonic acid-formaldehyde condensate, and the mixture is milled in a mechani caI mill. After 8 parts 15 by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising machine. A dust-free and free-fIow ing product wh ich is readily dispersible in wa ter is obtained in this manner.
ExampIe 7 parts by weight of 2-(ethylthi o-me thyl-phenyI ) N-methyI-carbamate are mixed intensively with 10 parts by weight of adipic acid, 9 parts by weight of magnesium carbonate, 10 parts by weight of mont mor illonite, 31 parts 25 by weight of kaol in and 15 parts by weight of a condensation product of cycI ohexanone, formaldehyde and sodium bisulphite, and the mixture is milled in a mechan i caI mi I I . After 8 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is 30 converted to layered granules in a pelletising machine.
A dust-free and free-flow ing product wh ich is readily dispersible in water is obtained in this manner.
ExampIe 8 parts by weight of 2—(ethyl thio-me t hyI -ph enyI ) 35 N-methyI-carbamate are mixed intensively with 10 parts by weight of adipic acid, 9 parts by weight.of magnesium 1- «! _ U - "" " ' <J/ '• carbonate, 10 parts by weight of montmori I I oni te, 31 parts by weight of kaol in and 15 parts by weight of a condensation product of cycI ohexanone, formaldehyde and sodium bisulphite, and the mixture is milled in a mechan i caI 5 mi I I . After 8 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising ma chine. A dust-free and free-flow ing product which is readily dispersible in water is obtained in this manner. 1 0 ExampIe 9 parts by weight of /S-fr, 1 '-b iphenyl )-4-yloxy3~ o(- ( 1 , 1 -d i me thyl ethyl ) — 1 H — 1 , 2,4-triazol e-1-ethanol are mixed intensively with 3 parts by weight of a wetting agent based on a I ky I a ryl-su Iph ona t e , 20 parts by weight 15 of diphenyl ether-suIphonic acid-formaldehyde condensate, 15 parts by weight of adipic acid, 7 parts by weight of sodium bicarbonate and 30 parts by weight of si I it resin (inert), and the mixture is milled in a mechanical mill. After 6 parts by weight of water have been added and 20 thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising mach i n e. A dust-free and free-flow ing product wh ich is readily dispersible in water is obtained in this manner.
ExampIe 10 25 parts by we ight of B - (£1 , 1 ' -b i phenyI )-4-yIoxyj- q(- ( 1 , 1 -d i me thyl)-1H-1,2,4-triazole-1-ethanol are mixed intensively with 20 parts by weight of diphenyl ether-sulphonic acid-formaIdehyde condensate, 15 parts by weight of adipic acid, 7 parts by weight of sodium bicarbonate 30 and 33 parts by weight of si Iit resin (inert), and the mixture is milled in a mechanical mill. After 6 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising ma chine. A dust-free and free-flow i ng 35 product wh ich is readily dispersible in wa ter is obtained in this manner. - 1 5 - ExampIe 11 parts by weight of/S-{(l,1'-biphenyl)-4-yloxy]-$(- ( 1 , 1 -d i me thyl)-1H-1,2,4-triazole-1-ethanol are mixed intensively with 20 parts by weight of a dispersing 5 agent based on I ignin-suIphonate, 15 parts by weight of adipic acid, 7 parts by weight of sodium bicarbonate and 33 parts by weight of si lit resin (inert), and the mixture i s m i I Ied i n a mechan ical mill. After 6 parts by weight of water have been added and thorough mixing has been 10 effected, the pre-mix is converted to layered granules in a pelletising ma chine. A dust-free and free-flowing product wh ich is readily dispersible in wa ter is ob t a i n ed in this manner.
ExampIe 12 50 parts by weight of acetyl-salicylie acid are mixed intensively with 5 parts by weight of citric acid, 5 parts by weight of sodium bicarbonate and 40 parts by we ight of lactose, the mixture is milled in a mechanical mi I I . After 6 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising ma chine. A dust-free and free-flowing product which is readily dispersible in water is obtained in this manner.
ExampIe 13 50 parts by weight of acetyl-salicylie acid are mixed intensively wi th 5 parts by weight of citric acid, 5 parts by weight of sodium bicarbonate and 40 parts by we ight of rice starch, and the mixture is milled in a mechan ical mill. After 6 parts by weight-of wa ter have 30 been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising machine. A dust-free and free-flowing product which is readily dispersible in wa ter is obtained in this mann e r. ExampIe 14 50 parts by weight of acetyl-salicylie acid are mixed intensively with 5 parts by weight of citric acid, iV«I 2i"ha»'r8t 2031 parts by weight of sodium bicarbonate, 40 parts by weight of lactose and 5 parts by weight of vitamin C, and the mixture is milled in a mechanical mill. After 6 parts by weight of water have been added and thorough 5 mixing has been effected, the pre-mix is converted to layered granules in a pelletising machine. A dust- free and free-flow ing product wh ich is readily dispersible in water is obtained in this manner.
ExampIe 15 80 parts by weight of the oil-soluble dyestuff Ceres Red G are mixed intensively with 5 parts by weight of adipic acid, 5 parts by weight of sodium bicarbonate and 10 parts by weight of sulphite waste liquor, and the mixture is milled in a mechan ical mill. After 6 parts 15 by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising machine. A dust-free and free-flowing product which is readily dispersible in water is obtained in this manner.
ExampIe 16 70 parts by weight of a water-soluble azo dye-stuff are mixed intensively with 5 parts by weight of adipic acid, 5 parts by weight of sodium bicarbonate and 20 parts by weight of sulphite waste liquor, and the mix-25 ture is milled in a mechan ical mill. After 6 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules in a pelletising machine. A dust-free and free-flowing product which is readily dispersible in water is 30 obtained in this manner.
ExampIe 17 parts by weight of 1 -(4-chIorophenoxy)-3,3-dimethyI - 1 -(1,2,4-1riazoI-1-yI )-butan-2-one are mixed intensively with 20 parts by weight of sulphite waste 35 I iquor, 10 parts by weight of succinic acid, 5 parts by weight of magnesium carbonate, 10 parts by weight of 2031 2 - 1 7 - mon t morillonite and 50 parts by weight of kaolin, and the mixture is milled in a mechan ical mill. After 7 parts by weight of water have been added and thorough mixing has been effected, the pre-mix is converted to layered granules 5 in a tabletting machine. A dust-free and free-flowing p rodu c t wh ich is readily dispersible in wa ter is ob t a i n ed in this manner.
ExampIe 18 parts by weight of 1 -(4-chI orophenoxy)-3,3-10 dimethyI - 1 -(1,2,4-1riazoI-1-yI )-butan-2-one are mixed intensively with 20 parts by weight of sulphite waste liquor, 10 parts by weight of succinic acid, 5 parts by weight of magnesium carbonate, 10 parts by weight of mon t mor illonite and 30 parts by weight of kaolin, and the 15 mixture is milled in a mechan ical mill. After 7 parts by weight of water have been added and thorough mixing has been effected, the pre-mix i s converted to I ayered granu I es in a tabletting machine. A dust-free and free-flowing p rodu c t wh ich is readily dispersible in wa ter is obtained 20 in this manner.
ExampIe 19 parts by weight of 1-(4-chIorophenoxy)-3,3-d i me thyl-1-(1,2,4-triazol-1-yl)-butan-2-one are mixed intensively with 20 parts by weight of sulphite waste 25 liquor, 10 parts by weight of itaconic acid, 5 parts by weight of magnesium carbonate, 10 parts by weight of mon tmor illonite and 50 parts by weight of kaolin, and the mixture is milled in a mechan ical mill. After 7 parts by weight of water have been added and thorough mixing 30 has been effected, the pre-mix is converted to layered granules in a tabletting machine. A dust-free and free-fIow ing product wh ich is readily dispersible in wa ter is obtained in this manner.
ExampIe 20 5 parts by weight of 1-(4-chIorophenoxy)-3,3- d i me thyl-1-(1,2,4-triazol-1-yl)-butan-2-one are mixed

Claims (13)

# 27 ..o - 18 - intensively with 20 parts by weight of sulphite waste liquor, 10 parts by weight of succinic acid, 5 parts by weight of magnesium carbonate, 10 parts by weight of montmori I I oni te and 50 parts by weight of kaol in, and the 5 mixture is milled in a mechan ical mill. After 7 parts by weight of water have been added and thorough mixing has been effected, the pre-mix i s converted to layered granules in a tabletting machine. A dust-free and free-flowing product wh ich is readily dispersible in wa ter is obtained 10 'n this manner. uftnuiu. ia ..va-4 -19- 203127 WHATWWE CLAIM IS:
1. Water-dispersible or water-soluble granules containing (1) 5 to 80% by weight of at least one active component (2) 5 to 30% by weight of at least one product capable of producing gas, (3) 2 to 60% by weight of one or more additives, and,if necessary, (4) 1 to 20% by weight of granulating liquid, the sum of the constituents being 100% by weight in each case.
2. Granules according to claim 1, in which as the active component (1) is one or more substances selected from agrochemical active compounds, active compounds for combating pests in the household field and hygiene field, pharmacologically active substances,and dyestuffs.
3. Granules according to claim 1 or 2, in which the r-is product capable of producing gas (2)\one or more compounds or compositions selected from mixtures of an acid and a carbonate, mixtures of an acid anhydride and a carbonate, substances which split off nitrogen, and mixtures which consist of bacteria and lactic acid and are capable of producing carbon dioxide.
4. Granules according to any of claims 1 to 4, in which the additive(s) (3) is or are selected from surface-active substances, dispersing agents, extenders, binders , preservatives and dyestuffs.
5. Granules according to any of claims 1 to 5, in which the granulating liquid (4) is water, at least one organic solvent, or a mixture of water and at least one organic solvent.
6. Granules according to claim 5, in which the organic solvent is an alcohol, a halogenohydrocarbon or an ether.
7. Granules according to claim 5, in which the granulating liquid (4) is water. 203127 -20-
8. Granules according to any of claims 1 to 7 containing (1) 10 to 70% by weight of the at least one active component, (2) 10 to 28% by weight of the at least one product 5 capable of producing gas, (3) 5 to 50% by weight of the one or more additives, and, if necessary, (4) 3 to 8% by weight of the granulating liquid, the sum of the constituents being 100% by weight in 10 each case.
9. Granules according to claim 1, as described in any one of Examples 1 to 20.
10. A process for the production of granules according to any of claims 1 to 9, in which 15 (a) at least one active component (1) is mixed with at least one product (2) capable of producing gas, and with additive(s) (3), (b) the resulting mixture is finely milled, thereafter granulating liquid is added, and the mixture is dried 20 if desired and (c) the mixture is pelleted or tabletted, the constituents being added in amounts such that the / 30% bv weight of con.q-H t-npnt-granules contain 5 to 80% by weight of constituent (l)" 5 to| (2), 2 to 60% by weight of additive(s) (3) and 1 to 25 20% by weight of granulating liquid (4), with the sum of the constituents being 100% by weight in each case, and the active component, if liquid at room temperature, having been absorbed, before granulation,on a solid carrier. 30
11. A process for the production of granules according to claim 1, substantially as described in any one of Examples 1 to 20.
12. Granules according to claim 1 whenever produced by the process of claim 10 or 11. 35 Iaj A 21 ^ /v 30 MAY 1985^ ^ // I \J 203127 -21-
13. Use of granules according to any of claims 1 to 9 and 12 for plant protection in agriculture and in horticulture, for combating pests in the household field and hygiene field, for combating diseases or for dyeing with the proviso that the use does not include a method of treatment of the human body. BAYER AKTIENGESELLSCHAFT By Their Attorneys HENRY HUGHES LIMITED By:
NZ203127A 1982-02-02 1983-01-31 Water-dispersible or water-soluble granules their production and use NZ203127A (en)

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AU5755986A (en) * 1985-05-20 1986-11-27 Autotrol Corporation Soluble polymeric material matrix + water treating material
GB8600190D0 (en) * 1986-01-06 1986-02-12 Microbial Resources Ltd Pesticidal formulations
US4933000A (en) * 1987-10-05 1990-06-12 Ciba-Geigy Corporation Herbicidal compound concentrate
US5348745A (en) * 1989-05-09 1994-09-20 Miles Inc. Aqueous granulation solution and a method of tablet granulation
CA2009326C (en) * 1989-05-09 1998-01-27 Lawrence J. Daher Aqueous granulation solution and a method of tablet granulation
JP2907299B2 (en) * 1989-09-07 1999-06-21 ゲルゲリイ、ゲルハルト Pharmaceutical preparations that bind stomach acid
RU2126207C1 (en) * 1991-02-06 1999-02-20 Хехст АГ Pesticide substance in the form of water-emulsifiable granulate
ZA93400B (en) * 1992-01-24 1993-08-05 Ici Australia Operations Water dispersible granules of liquid pesticides.
WO1995003785A1 (en) * 1993-08-03 1995-02-09 Warner-Lambert Company Pleasant tasting effervescent cold/allergy medications
DE4420735C2 (en) * 1994-06-15 1996-09-05 Allphamed Arzneimittel Gmbh Process for the production of mechanically stable, high-speed effervescent tablets
DE19632928A1 (en) * 1996-08-16 1998-02-19 Bayer Ag Process for the preparation of inorganic granules and their use

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FR1042960A (en) * 1950-05-10 1953-11-05 Gen Aniline & Film Corp Water-dispersible coloring matter powders
GB847370A (en) * 1955-12-02 1960-09-07 Donald Philip Henry Josephs Improvements in or relating to preparations for herbicidal, insecticidal or fertilizing purposes
FR1397117A (en) * 1962-07-25 1965-04-30 Dausse Soc Lab Process for preparing a homogeneous and stable mixture of dipiproverin dihydrochloride and sorbitol
FR2044216A5 (en) * 1969-05-12 1971-02-19 Ile De France Effervescent tablets prepd by aqueous - granulation
GB1357813A (en) * 1970-09-07 1974-06-26 Siphar Sa Effervescent composition for the treatment of heart diseases
CA986416A (en) * 1971-09-08 1976-03-30 Dolores T. Kenney Bath preparation compositions which dissolves with effervescence
IT1025700B (en) * 1974-11-14 1978-08-30 Montedison Spa PESTICIDE GRANULATES ACT IN WATER
US4115307A (en) * 1974-12-13 1978-09-19 Erco Industries Limited Phosphate composition
FR2316921A1 (en) * 1975-07-08 1977-02-04 Blendax Werke Schneider Co Dentrifice cleaning compsn in tablet/powder form - contains urea and acts rapidly
GB2095556A (en) * 1981-03-30 1982-10-06 Alza Corp Sterilization composition
DE3128162A1 (en) * 1981-07-16 1983-02-03 Happel, Fritz, 8951 Baisweil COMBINED CONTROL AND COLLECTING PIECE FOR MACHINE MILKING DEVICES

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PT76137A (en) 1983-02-01
ES8405054A1 (en) 1984-05-16
EP0085376A2 (en) 1983-08-10
ES519421A0 (en) 1984-05-16
ZA83650B (en) 1983-10-26
BR8300507A (en) 1983-11-08
DE3203443A1 (en) 1983-08-11
EP0085376A3 (en) 1984-09-05
JPS58133827A (en) 1983-08-09

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