CN1988799A - Process for producing a granular agrochemical composition - Google Patents
Process for producing a granular agrochemical composition Download PDFInfo
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- CN1988799A CN1988799A CNA200580024955XA CN200580024955A CN1988799A CN 1988799 A CN1988799 A CN 1988799A CN A200580024955X A CNA200580024955X A CN A200580024955XA CN 200580024955 A CN200580024955 A CN 200580024955A CN 1988799 A CN1988799 A CN 1988799A
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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
- A01N25/14—Powders or granules wettable
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
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- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
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Abstract
A water dispersible granular composition containing an agrochemical active agent, particularly a low use-rate active, and a particular basic, inorganic salt wherein a 1% aqueous solution of the composition has a pH of at least 8.0, and which is made by extruding a premix in the form of a free-flowing powder and without forming a paste provides improved bioavailability of the active. The invention is particularly useful in improving delivery of active from compositions having mixed actives and low levels of sulphonamide active.
Description
The present invention relates to a kind of new chemistry of pesticide composition and use thereof.The present invention relates more specifically to a kind of composition that contains agricultural chemicals and alkaline, inorganic salts, can effectively reactive compound be transported to the thing that is applied of desire processing.
The composition that contains bioactive compound is general to be required to be applied thing, for example crop with what active component was transported to that desire handles.Described conveying usually occurs in the aqueous environment, for example by will prepare wherein that composition of active components is disperseed and optional dissolved is administered to and is applied thing in water and with solution or dispersion.In the process of conveying active, composition can be scattered in the water-bearing media usually, if it is soluble, can begin dissolving, and therefore the speed of dispersion and dissolving and degree may influence the thing that is applied that active component all is transported to the desire processing.Active component can also solid form be applied to and be applied near thing or its, then with aqueous solution.Therefore, solid pesticide compositions can be applied to the place that plant or desire are handled, then water be added in the agricultural chemicals to dissolve on the spot and/or to disperse this agricultural chemicals.
When the dissolving of composition or disperse when incomplete, all dosage of active agent is failed to be transported to its target and is applied thing in the composition.Therefore, the dosage with the active component that is transferred may be lower than expection and can utilize mode to arrive the actual dose that is applied thing with biology uncertain.Therefore, may need to use higher dosage obtaining certain effect, but the actual dose of carrying is still uncertain, the product consumption may be insufficient, has illeffects and cost is higher, because active component generally is a composition the most expensive in the composition.In addition, uncertain may the causing that is applied the dosage of thing for the target that arrives expection left over the remaining active agent of not carrying near it uses ground, thereby may cause environmental nuisance or bad local concentration.
In case be mixed with preparation, composition pesticide also should be reasonably suitably keeping sufficient chemistry and physical stability in the time span, so that can make the product that will store and disperse not have the degraded of essence.
WO01/13721 discloses a kind of water-dispersible pesticide composition, contains the pesticide activity component of low consumption, and its content is 50% and a kind of dispersant that is lower than composition weight, and suitable is nonionic or anion surfactant.Compare with previous known composition, the compositions display of WO01/13721 goes out good conveying characteristic, and sufficient stability is provided.
Yet, still be desirable to provide the further conveying that improves active component, with bioavailability therefore, the stability of not sacrificing product simultaneously to be to reduce or to avoid above-mentioned defective, particularly dissolve in water-bearing media or disperses under the situation of deficiency at composition or active agent.Except the composition of product, the method for its combination may there be remarkable effect to the conveying of active component.
We have now found that by alkaline, inorganic salts is combined with pesticide activity component so that alkaline solution is provided when composition dissolves and avoids forming paste before extruding composition is with the formation particle, can obtain the composition pesticide that conveying characteristic improves, particularly the water-dispersible granule made from extrusion method.We find that also described particle demonstrates acceptable stability.In addition, we find that particularly for the composition that contains the combination of low-level pesticide activity component or active component, transportation performance improves, and can be after dissolving the previously known more a high proportion of active component of delivery ratio in a short time.
Therefore, first aspect present invention provides a kind of preparation method who contains pesticide activity reagent and the alkaline, inorganic salts and the particulate composition of the dispersant of choosing wantonly, wherein the pH value that 1% aqueous solution of said composition has when carrying out CIPAC TestMT75.3 is at least 8.0, this method comprises the pre-composition that forms free-pouring powder form, stick with paste but not form, this pre-composition contains active component, alkaline, inorganic salts and optional dispersant, at least a in the composition of pre-composition is liquid, extrudes this pre-composition to form particle and this particle of optionally drying.
The present invention helps to strengthen the conveying of the pesticide activity component in the water-dispersible particulate composition especially.
Second aspect, the invention provides a kind of speed and degree methods that pesticide activity component dissolves that increase in water-bearing media, this method comprises that preparation contains the composition of pesticide activity component and alkaline, inorganic salts, so that the pH value that 1% aqueous solution of said composition has when carrying out CIPAC Test MT75.3 is at least 8, with describedly have the pre-composition of active component and described salt and optional dispersant suitably to make composition by extruding to contain, wherein before extruding, do not form paste.
Composition in the second aspect present invention is suitably made by a kind of method, described method comprises the pre-composition that forms the free-pouring powder form contain active component, alkaline, inorganic salts and optional dispersant, and do not form paste, wherein at least a in the composition of pre-composition is liquid, extrudes this pre-composition to form particle and this particle of optionally drying.
Third aspect present invention provides the application of alkaline, inorganic salts in composition pesticide, with the solvability of enhanced activity composition when mixing with aqueous solution, improve thus active component is transported to the plant of desire processing or the conveying characteristic in place, described composition contains pesticide activity component and described salt, and suitably makes by the extrusion method that does not form paste before extruding.
As the increase of the increase of the dissolution velocity of the described composition of second aspect present invention and degree or the described active component solvability of third aspect present invention will with the same terms under contain with the dissolution velocity and the degree of the identical component of present composition par and the comparative composition by the same procedure manufacturing and compare, just this comparative composition contains inert filler such as starch commonly used in the pesticidal preparations, lactose, china clay and kaolin replace inorganic alkaline salt, and described filler makes the pH that 1% aqueous solution of comparative composition has when carrying out CIPAC Test MT75.3 be lower than 8.
By in composition, mixing alkaline, inorganic salts, the pH that 1% solution of composition provides is at least 8, preferably at least 8.5, particularly at least 9, stick with paste with avoiding before extruding, forming, dissolution velocity and the degree of active component in the aqueous solution can increase, thereby outstanding active component bioavailability is provided.
The present invention is specially adapted to the pesticide activity component of low consumption, because of its usually may be under service condition solvability in water or bad dispersibility, for example bensulfuron-methyl.When using in this article, term " low consumption " active component is represented be lower than the pesticide activity component of using under the consumption of 100g/ha usually, and term " high consumption " active component is represented be higher than the pesticide activity component of using under the 1000g/ha consumption usually.
Suitable low consumption pesticide activity component comprises Olivomitecidin, Fluoxastrobin, bensulfuron-methyl, carfentrazoneethyl, green sulphur is grand, cinosulfuron, alkynes grass ester, clopyralid, cyhalothrin, decis, Diflufenican, emaricin, fluorine worm nitrile (fibronil), the fluorine humulone, miaow grass ester, the weed eradication cigarette, Imazethapyr, Imidacloprid (imadacloprid), metsulfuron-methyl, more visit rhzomorph (milbectin), nicosulfuron, primisulfuronmethyl (pirimisulfuron-methyl), rimsulfuron 25, Sulfometuron Methyl, thifensulfuron methyl, tribenuron-methyl, and triflusulfuronmethyl.Preferred low consumption active component comprises sulfonylureas, and for example bensulfuron-methyl and chlorine sulphur are grand.
The content of pesticide activity component carries out suitable selection according to the particular compound and the using of expection of using.For low consumption active component, concentrate composition can be used for high level to be used, 60g/ha at least for example, and composition is suitable to contain at least 10%, preferably at least 50% active component, particularly 50-70% active component.When requiring low-level using, for example be lower than 50g/ha, composition suits to contain to be lower than 10% active component, preferably is lower than 7% active component, particularly the 1-7% active component.Suitable is that the level of the active component that composition contains should can provide its concentration that the activity component concentration of beneficial effect can be provided when plant of handling the desire processing or place when for example water mixes with liquid-carrier.
Composition dissolving rapidly in aqueous environment made in accordance with the present invention forms the solution of active substance, and the ratio of active component is higher than the active component that contains par but replaces the composition of alkaline, inorganic salts with inert filler in the solution.This characteristic has strengthened the effectiveness of active agent by the conveying in the plant of improving active component and handling to desire or place.The bioavailability of this enhancing represents can obtain by the active component that uses the total amount lower than expection the effect of active agent.For agricultural chemicals, the effect that obtains setting by lower consumption is favourable to environment.
Practical advantage provided by the invention is can contain in the composition active component of reduced levels, and because the higher proportion dissolving still can be carried the active component of setting dosage.In addition, the active component level is lower than the conventional levels of the active component that obtains the setting delivered dose in composition, and the risk that some active component is not dissolved in liquid-carrier reduces.Therefore, can reduce the risk that causes the high local concentrations active component owing to poor dissolution in aqueous environment.The high local concentrations active component that may cause crop damage is to crop, and particularly the infiltration of plant root can be lowered.
Another advantage is to compare with the conventional composition that uses high-level active component, and the active component of reduced levels has strengthened the flexibility in compositions formulated.Therefore, formulator can comprise in composition that other materials of second kind of active component or needs are to provide the balance of optimum efficiency or performance.
Alkaline, inorganic salts is suitably alkali metal salt, for example sodium salt and sylvite.The anion of this salt can be to prepare so that bioactive composition to be provided with the active component of selection when this salt, and 1% aqueous solution of said composition has any anion of at least 8 pH value according to CIPAC Test MT75.3 test.In preferred embodiments, alkaline, inorganic salts comprises alkali carbonate, phosphate, bicarbonate, hydrophosphate, trimetaphosphate, hexametaphosphate, polyphosphate, tripolyphosphate and pyrophosphate.Preferred especially potash and sodium carbonate.Alkaline, inorganic salts can be ground to the particle diameter that needs as required, 1-20 micron for example, the dissolubility of proportionately giving composition for improved.
The suitable content of alkalescence inorganic matter is at least 1%, aptly preferably at least 3%, and this salt content is no more than 40% and preferably be no more than 30%.
Find in composition, to use anhydrous salt that outstanding dissolubility can be provided, but can not cause the chemistry of composition or the unacceptable deterioration of physical stability.Suitable is that the present invention contains anhydrous alkaline, inorganic salts, preferred anhydrous sodium salt, for example natrium carbonicum calcinatum.If if alkaline, inorganic salts is not moisture or moisture, water content is no more than 2wt%, think that then this salt is anhydrous.
The example of particularly preferred active agricultural chemicals and alkaline, inorganic salts combination comprises the grand and sodium carbonate of bensulfuron-methyl and sodium carbonate and chlorine sulphur.Suitable is that sodium carbonate is anhydrous.
For containing the known compositions that is lower than 10% active component, after 5 ℃, 15 minutes the amount of active component of dissolving with composition in the percentage of active principle represent to be usually less than 65% or even be lower than 50%.
Account for composition weight at the most for the composition of 10% active agent for containing made in accordance with the present invention, suitable is in the composition at least 70% of active agent, aptly 80%, preferably at least 90% after 5 ℃, 15 minutes, be dissolved in the water.Preferred at least 60% or preferably at least 70% active component dissolved after 5 minutes.Best is, for composition made in accordance with the present invention, and the ratio height at least 30% of the active component that after 5 ℃, 15 minutes, dissolves in the ratio comparative composition of the active component of dissolving, aptly at least 45%.
In known composition pesticide, for containing at least 50% composition of active components, after 5 ℃, 15 minutes the amount of active component of dissolving with composition in the percentage of active principle represent to be usually less than 20% or even be lower than 15%.Suitable is, is higher than 10% and preferably be higher than 50% composition of active components for containing, and in the composition at least 25% of active component, wishes that at least 40% and preferably at least 70% dissolves after 5 ℃, 15 minutes.Preferably at least 40% dissolving after 5 minutes.Best is, for composition made in accordance with the present invention, and the ratio height at least 100% of the active component that after 5 ℃, 15 minutes, dissolves in the ratio comparative composition of the active component of dissolving, aptly at least 200%.
The dissolving of composition can be by described method test under " dissolubility data " title among the embodiment.
The total pesticide activity component and the weight ratio of alkaline, inorganic salts preferably are no more than 10: 1 in the composition, are no more than 6: 1 aptly.The pesticide activity component that preferred composition is total and the weight ratio of alkaline, inorganic salts are at least 1: 3, aptly at least 1: 1.In preferred embodiments, this ratio is 1 to 12: 2, more preferably 1 to 6: 1.Best is, is lower than total composition of active components of 10% for containing, and total content of active component is not less than alkaline, inorganic salts, most preferably 4 to 1: 1.Greater than 10% composition, the total content of active component is 4 to 2: 1 with the ratio of alkaline, inorganic salts aptly for gross activity composition level.For example, the composition the best with total activity level of 5% contains the inorganic alkaline salt of about 1-5% level, and the composition the best with total activity level of 60% contains the inorganic alkaline salt of composition weight 15-30%.
Composition can cause single active component to use under low consumption and phytotoxicity is lower than the conventional composition of described active substance made in accordance with the present invention, can resist various pests and disease.
In preferred embodiments, composition contains second kind of active component.In preferred embodiments, second kind of active component that active component is high consumption.Suitable high consumption active component comprises atrazine, benomyl, bentazone, bifenox, Brominal, captan, carbendazim, pyrazone, tpn, chlortoluron, plictran, frost urea cyanogen (cymoxynil), the nail body cypermethrin, decis, dimethomorph, diuron, ethofumesate, glyphosate, miaow grass ester, the weed eradication cigarette, Imazethapyr, isoproturon, lorox, mancozeb, maneb, metamitron, methiocarb, the piperazine humulone, Oxyfluorfen, phenmedipham, Stam F-34, pentyne grass amine, Simanex and tmtd.Preferred high consumption active component comprises Stam F-34 or isoproturon.
The example of the combination of particularly preferred high consumption, the active agricultural chemicals of low consumption and alkaline, inorganic salts comprises bensulfuron-methyl, Stam F-34 and sodium carbonate, and chlorine sulphur is grand, isoproturon and sodium carbonate.It is anhydrous that sodium carbonate is suitably.
The content of high consumption active component is suitably at least 30% of composition weight, and more preferably at least 50%, the best at least 65%, for example 75%.
Aptly, composition comprises dry granular formulations free-pouring, dustless and that dissolve rapidly.
Second kind of active component can add in the pre-composition that first kind of active component arranged or active component can add as required in proper order.
Composition is suitable to contain dispersant to help rapid dispersion and dissolving and composition the using subsequently of active substance when the dilution.The weight ratio of dispersant and active component is suitably 0.1 to 10: 1 in the composition, and preferred 0.4 to 6: 1, for example about 4: 1 and about 5: 1.
In preferred embodiments, dispersant comprises surfactant, preferred nonionic surfactants, particularly anion surfactant.The example of suitable dispersant comprises the alkali metal salt of lignosulfonates, particular certain cancers, naphthalenesulfonate formaldehyde condensation compound, tristyrylphenol ethoxylates phosphate, aliphatic alcohol ethoxylate, alkylphenol ethoxylate, ethylene oxide/propylene oxide (EO-PO) block copolymer, " comb " shape graft copolymer and polyvinyl alcohol-vinyl acetate copolymer.Other dispersants known in the art can use as required.
The suitable eletrokinetic potential that has of dispersant is about 0mV for non-ionic surface active agent, for anion surfactant suitable be to surpass-30mV, be to surpass+30mV for cationic surfactant.
Except that dispersant, can there be other compositions, for example wetting agent in the composition.Suitable wetting agent comprises: the alkali metal salt of alkylaryl sulfonate, alkaryl sulfosuccinate and alkyl sulfate, particular certain cancers.
Other wetting agents well known by persons skilled in the art and other excipient can adopt as required, comprise disintegrant, for example bentonite, modified starch and polyvinylpyrrolidone; Stabilizing agent, for example citric acid, polyethylene glycol and Yoshinox BHT; And filler, for example starch, lactose, china clay, sucrose and kaolin; And glidant.Preferred composition contains filler, for example to dissolving useful lactose and helping the composition of composition to extrude the lactose of formation particle and the mixture of china clay.
Preferably by the preparation of method described in the EP-A-1161145, its content is incorporated herein by reference composition of the present invention.The suitable mixture that comprises preparation free flowing powder form of this method; Be preferably uniform powder, contain active component and alkaline, inorganic salts and optional dispersant and do not form other compositions of paste, and for example extrude this pre-composition in the low pressure extruder at extruder and form particle, preferably do not form paste, this particle is chosen wantonly and is dried.Optional other compositions that contains of pre-composition, for example second kind of active component can mix the mixture to be formed for extruding with active component and alkaline, inorganic salts.Suit to contain liquid component, and can use liquid dispersant, although can comprise other liquid component as required in this case, other liquid component is optional.If in pre-composition, added entry, can remove by drying so.
The device that is applicable to blend step comprises the high-intensity blender of low-shearing force, as LodigePloughshare blender, ribbon mixer, Y-cone blender, bipyramid drum mixer or trough mixer, so that form free-pouring powder.Mixture directly or indirectly is fed in the suitable low pressure extruder,, thereby makes pre-composition be compacted and form particle by aperture at the aperture place of screen cloth for example as described in the WO96/26828.
In preferred embodiments, the setting of the composition of mixture and extruder should be able to be avoided before extruding forming and stick with paste and the state of processed material maintenance free flowing granule thing in the process that forms pre-composition and during extruding aptly.Do not form paste before particularly material is preferably in and extrudes.Yet because composition can contain one or more liquid components, therefore as long as it keeps free-flowing and graininess in process, it can be that wet or dried.About this point, paste can see to get into a clinch and contain the material of sufficient liquid, agglomerate for example, or processed particulate material forms plastic or deformable and can not free-pouring agglomerate under said temperature.Therefore, sticking with paste can be for example by friction disintegration beading between finger when applying shearing force, but still keeps the bulk of caking, and the shearing force effect only can the mold pressing agglomerate or made the agglomerate distortion.
If desired, can be earlier with each composition of composition successively, simultaneously or part successively with other simultaneously in for example stirrer for mixing, obtain uniform mixture, thus then with it by suitable crushing system such as windmill, pin mill or air swept mill obtains fine powder
*(pre-composition), the suitable average grain diameter of this fine powder is 0.5-20 μ m, or more preferably 0.5-5 μ m.So the powder that obtains is preferably by the suitably agglomeration of the described method of EP-A-1161145, to obtain evenly dustless particle.This method for optimizing for example is included under the described low temperature of EP-A-812256 and extrudes wet-milling in the low pressure extruder, and the wet-milling of this moment is the form of free flowable uniform powder.
At present, low consumption and high consumption agricultural chemicals can be in the processes that forms the dry pre blend thing and other preparation compositions dispersant for example, and perhaps as an alternative, available a kind of agricultural chemicals prepares pre-composition, and another kind is added in the pre-composition after grinding.When high consumption agricultural chemicals was Stam F-34, this replacement method was preferred, and Stam F-34 is fit to mix in the dry pre blend thing, added low consumption agricultural chemicals then in pre-composition, and mixed with it before granulation.
On the other hand, the invention provides and a kind ofly be administered to plant or plant location methods for the treatment of plants by composition made in accordance with the present invention with herbicidally effective amount.
The present invention can make the present composition at the consumption lower than known compositions, and promptly the composition quality that unit are is lower uses and the predetermined effect of acquisition down.With agricultural chemicals be administered to plant or the on-site suitable consumption of plant be lower than active component in the commercially available composition conventional amount used 75%, more preferably less than 50%.
In preferred embodiments, contain the low consumption active component of sulfonylureas for example the composition of bensulfuron-methyl use with the consumption that is lower than the 50g/ hectare, particularly be lower than the 30g/ hectare, best for being lower than the 20g/ hectare.Usually, commercially available contain can the 60g/ hectare above the composition of the bensulfuron-methyl of composition weight 50% or higher consumption use.In another preferred embodiment, in the composition except that sulfonylureas active substance for example the bensulfuron-methyl, also contain the second kind of active component of high consumption that comprises Stam F-34, second kind of active component suits to use with the consumption that is lower than the 7000g/ hectare, preferably be lower than the 5000g/ hectare, particularly be lower than the 3200g/ hectare.
When plant was weeds, suitable was that processing is in order to control or kill weeds.Usually utilizing liquid-carrier, generally is water, and composition is administered to plant or its location, and wherein composition mixes with liquid-carrier before using.If desired, composition can be mixed formation with liquid-carrier and be applicable to the concentrate that mixes with liquid-carrier subsequently.The composition of solid or concentrate form is administered to plant or its location, when especially near plant, having water to exist, also within the scope of the invention by natural sedimentation.
Composition suits to be diluted to the concentration of 10-500mg/l and preferred 20-300mg/l so that use in water.Dilution factor suits according to compositions for use, the type of using, needs growth conditions and other factors well known by persons skilled in the art of the plant of processing to select.
The present invention relates to make method for compositions and methods for the treatment of plants, for example kill or control weeds by using than active component (suitably dilution back in water) with the lower consumption of the routine suggestion consumption of described active component antagonism weeds.In addition, the present invention can avoid the subsequent applications of described active component, has therefore further reduced the consumption of agricultural chemicals.
The present invention describes by following non-restrictive example.
Embodiment 1-8 and Comparative Example A An-C
Mix until evenly by the active component and the GALORYL DT505 (a kind of naphthalene sulfonic acids) that will pulverize earlier, use the Gem-T pneumatic grinding mill to pulverize then and prepare of the present invention a series of compositions with the listed prescription of table 1.Add sodium carbonate and filler to this premix species, and in super mixer, mix until evenly.When mixing, add distilled water based on mixture weight 12%.The wet pre-composition of free flowing powder form is dosed to the described box extruder as EP-A-812256, by the 1mm screen cloth.Obtain extrudate closely, the gained particle was 60 ℃ of dryings 8 minutes.Do not form paste before extruding.Then with dried granules by 2mm and 500 tm screen mesh screen branches.
Use Hewlett Packard 1050 HPLC instrument to carry out assay determination.Use HPLCMethod LC29 to analyze.Use available from the analytical standard of QMx as the reference material.
The embodiment 3 that contains a galactose and half china clay is easier to extrude than embodiment 1 and 2.
Table 1
| Embodiment | Bensulfuron-methyl is analyzed (%) | Sodium carbonate (%) | Galoryl DT505(％) | Filler (surplus %) |
| 1 | 5 | 5 | 10 | Lactose |
| 2 | 5 | 2 | 10 | Lactose |
| 3 | 5 | 3 | 10 | Lactose/china clay (50/50) |
| 4 | 60 | 10 | 20 | Lactose |
| 5 | 60 | 15 | 10 | Lactose |
| 6 | 60 | 20 | 10 | Lactose |
| 7 | 60 | 20 | 12.5 | Lactose |
| 8 | 60 | 20 (pulverizing) | 12.5 | Lactose |
Use following method to determine the various physical characteristics of composition, the results are shown in following table 2.
Suspendability
0.5g product (being weighed into four decimals) joined in the 100ml graduated cylinder in 20 ℃ the 100ml running water to 100ml scale place.On graduated cylinder, place the graduated cylinder lid, and go back to totally 30 times again for 180 ° around the upset of graduated cylinder center.Reversal rate be per second once.If overturn after 30 times, product disperses fully, with 5 times one group further overturn and disperse until all products, or until finishing 60 upsets.
Make graduated cylinder leave standstill 30 minutes.The 50ml scale pipettes the 10ml dispersion and places and weighs in advance and dry evaporating dish from the graduated cylinder afterwards.Using water-bath to remove anhydrates.After all water evaporations, by 3 minutes further dry these wares of microwave moderate heat.Treat then to weigh once more after this ware is cooled to room temperature.
Formula below using calculates suspensibility:
Y
*=remaining the quality of 10ml running water when measuring
The remaining test of the merging wet screening of 75 μ m and 150 μ m sieve
5g product (being weighed into four decimals) is added in the 250ml beaker that contains the 100ml running water.Manually stir product, even or maximum 5 minutes until suspension.
Wetting in advance 75 μ m and 150 μ m sieve under tap.150 μ m sieve is placed on the 75 μ m sieves and with suspension pours into,, wash all residues with the running water of 3L/ minute flow velocity and reach 2 minutes by two sieves.Thoroughly clean beaker, guarantee that all contents all transfer on the sieve.
Separately two sieves use deionized water that the residue on each sieve is transferred in the predrying and preweighted evaporating dish in wash-bottle.Use the water-bath evaporation water.After all water evaporations, by 3 minutes further dry these wares of microwave moderate heat.Treat then to weigh once more after this ware is cooled to room temperature.
Formula below using calculates 150 μ m wet screening remnants:
Formula below using calculates 75 μ m wet screening remnants:
Dispersed
The 100ml running water is poured in the 100ml graduated cylinder.Add the 1.0g product rapidly, the graduated cylinder lid is placed on the graduated cylinder, go back to again 10 times for 180 ° around axle upset afterwards by the graduated cylinder center.After 10 times, product disperses fully if overturn, disperse until all products with 5 one group of continuation upsets, or until reaching 60 upsets.
Dispersed grade star system:
*-few or do not have particle point/spot
*-a small amount of point/spot
* *-many point/spots
* * *-be less than 5 not dispersed particles
* * * *-more than 5 dispersed particles not
Table 2
| Embodiment | Dispersed (number of upset) | Suspensibility (%) | Wet screening 75 μ m | Wet screening 150 μ m | Moisture content (%) | Analyze (%) |
| 1 | 25 * | 97 | 0.01 | 0.01 | 0.67 | 5.02 |
| 2 | 25 do not have * | 100 | 0.03 | 0.06 | 0.80 | 5.18 |
| 3 | 25 * | 94 | 0.01 | 0.03 | 1.00 | 5.20 |
| 4 | 40 ** | 97 | 0.03 | 0.08 | 1.20 | 59.73 |
| 5 | 50 ** | 100 | 0.01 | 0.01 | 1.09 | 60.35 |
| 6 | 50 ** | 95 | 0.02 | 0.03 | 1.51 | 60.03 |
| 7 | 60 ** | 96 | 0.06 | 0.08 | 0.89 | 59.34 |
| 8 | 60 ***/100 ** | 97 | 0.10 | 0.14 | 0.60 | 56.25 |
Embodiment 3 and 8 is carried out stability test, in this test, composition was stored for 2 weeks under the specified temp in airtight container.The results are shown in table 3.
Table 3
| RT | 37℃ | 54℃ | 25/40℃ | F/T | 5℃ | ||
| Embodiment 3 | Suspensibility (%) | 88 | 90 | 92 | 90 | 89 | 90 |
| Wet screening (150 μ m) (%) | 0.01 | 0.01 | 0.01 | 0.01 | 0.01 | 0.01 | |
| Wet screening (75 μ m) (%) | 0.01 | 0.02 | 0.01 | 0.04 | 0.02 | 0.02 | |
| Dispersed | 25 * | 25 * | 25 * | 25 * | 25 * | 25 * | |
| Moisture content (%) | 1.31 | 0.98 | 1.20 | 1.00 | 1.12 | 1.02 | |
| Analyze (%) | 5.13 | 5.18 | 5.12 | 5.14 | 5.21 | 5.09 | |
| Remaining active component (%) | 98.7 | 99.6 | 98.5 | 98.8 | 100.2 | 97.9 | |
| Embodiment 8 | Suspensibility (%) | 95 | 93 | 96 | 96 | 98 | 97 |
| Wet screening (150 μ m) (%) | 0.02 | 0.01 | 0.01 | 0.01 | 0.01 | 0.01 | |
| Wet screening (75 μ m) (%) | 0.03 | 0.01 | 0.01 | 0.01 | 0.02 | 0.01 | |
| Dispersed | 100 * | 100 * | 100 * | 100 * | 100 * | 100 * | |
| Moisture (%) | 1.80 | 1.22 | 1.89 | 1.21 | 2.03 | 1.49 | |
| Analyze (%) | 55.91 | 55.96 | 56.13 | 56.04 | 55.95 | 55.59 | |
| Remaining active component (%) | 99.4 | 99.5 | 99.8 | 99.6 | 99.5 | 98.8 |
These results prove that described composition remains on the acceptable level at the time in 2 weeks internal stability.
Dissolubility data
The dissolubility property of the test present composition.In order more also to have tested three kinds of known compositions.These three kinds of comparative composition are as follows:
Comparative Example A An:
LONDAX 60-contains the commercially available bensulfuron-methyl product of 60% bensulfuron-methyl, can buy from Du Pont.
Comparative Examples B:
| Composition | Trade name | ％w/w |
| Bensulfuron-methyl | 64 | |
| Naphthalene sulfonic acids | GALOROYL DT505 | 13 |
| Formaldehyde condensation products, sodium salt | GALOROYL MT704 | 1 |
| Lactose | Lactose | 22 |
Comparing embodiment C:
| Composition | Trade name | ％w/w |
| Bensulfuron-methyl | 5 | |
| Naphthalene sulfonic acids | GALOROYL DT505 | 30 |
| Formaldehyde condensation products, sodium salt | GALOROYL MT704 | 1 |
| China clay | China Clay GTY | 64 |
Comparative Examples B prepares according to the method identical with the present composition with C.
Solvability test is carried out in 1L jacket layer container, is cooled to 5 ℃ and use magnetic stirring apparatus to stir with maximal rate by cooling agent (the third-1, the 2-glycol/water).Measure 1L CIPAC D water, pour in the jacket layer container and also stir until reaching heat balance.Measure the pH and the record (CIPAC D water is 6.5) of water.Continuing to add the composition that desire is tested under the stirring condition then, and the beginning stop-watch.5, after 15,30 and 60 minutes, use syringe to take out the 2ml sample, filter with Whatman GF/A filter paper immediately, analyze the bensulfuron-methyl of dissolved in filtrate.
The result
4-6 is shown in the results are shown in of solubility test.
Table 4
| Test sample | Amount of application g/ha | The bensulfuron-methyl g/ha that uses | The bensulfuron-methyl % of dissolving | The bensulfuron-methyl g/ha of dissolving | |||
| 5 minutes | 15 minutes | 30 minutes | 60 minutes | ||||
| Comparative Example A An | 100 | 60.0 | 3.2 | 3.4 | 3.5 | 3.9 | 2.3 |
| Comparative Examples B | 100 | 60.0 | 14.9 | 15.5 | 16.3 | 15.0 | 9.0 |
| Comparing embodiment C | 300 | 15.0 | 63.3 | 63.1 | 62.7 | 63.2 | 9.5 |
Table 5
| Embodiment | Amount of application g/ha | The bensulfuron-methyl g/ha that uses | The bensulfuron-methyl % of dissolving | The bensulfuron-methyl g/ha of dissolving | |||
| 5 minutes | 15 minutes | 30 minutes | 60 minutes | ||||
| 1 | 300 | 15.0 | 97.1 | 96.7 | 96.9 | 97.4 | 14.6 |
| 2 | 300 | 15.0 | 75.8 | 88.0 | 90.2 | 93.0 | 14.0 |
| 3 | 300 | 15.0 | 70.1 | 96.8 | 98.3 | 99.0 | 14.9 |
| 4 | 100 | 60 | 41.2 | 50.5 | 52.1 | 52.9 | 31.7 |
| 5 | 100 | 60 | 57.6 | 74.3 | 78.4 | 79.7 | 47.8 |
| 6 | 100 | 60 | 67.9 | 85.8 | 89.5 | 91.5 | 54.9 |
| 7 | 100 | 60 | 66.2 | 86.8 | 90.8 | 92.6 | 55.6 |
| 8 | 100 | 60 | 65.3 | 96.3 | 98.2 | 97.8 | 58.7 |
The wet pre-composition that uses in the preparation of compositions to embodiment 8, the preparation before promptly extruding carries out further solvability test.The result is as follows.
Table 6
| The pre-composition of embodiment 8 | 100 | 60 | 83.8 | 90.6 | 93.6 | 96.5 | 57.9 |
After following table 7 shows solvability test in 60 minutes, the variation of pH in every kind of testing liquid.
Table 7
| Embodiment | Bensulfuron-methyl is analyzed (%) | Sodium carbonate (%) | Amount of application g/ha | Initial pH (CIPAC D water, 5 ℃) | Last pH (CIPAC D water, 5 ℃) |
| 1 | 5 | 5 | 300 | 6.60 | 9.55 |
| 2 | 5 | 2 | 300 | 6.40 | 8.50 |
| 3 | 5 | 3 | 300 | 6.40 | 9.10 |
| 4 | 60 | 10 | 100 | 6.40 | 8.60 |
| 5 | 60 | 15 | 100 | 6.70 | 8.80 |
| 6 | 60 | 20 | 100 | 6.50 | 8.95 |
| 7 | 60 | 20 | 100 | 6.40 | 9.00 |
| 8 | 60 | 20 (pulverizing) | 100 | 6.60 | 9.00 |
Claims (25)
1. method for preparing particulate composition, described composition contains pesticide activity component, alkaline inorganic carbonate and optional dispersant, pH when wherein 1% aqueous solution of said composition carries out CIPAC Test MT75.3 is at least 8.0, this method comprises the pre-composition that forms the free flowing powder form contain active component, alkaline, inorganic salts and optional dispersant surfactants, and do not form paste, at least a in the composition of this pre-composition is liquid, extrudes this pre-composition and forms particle and this particle of optionally drying.
2. method according to claim 1, wherein the alkaline, inorganic salts in the composition makes 1% aqueous solution of composition have at least 8.5 pH value.
3. method according to claim 1 and 2, wherein active component comprises low consumption pesticide activity component.
4. method according to claim 3, low consumption active component wherein comprises sulfonylureas.
5. method according to claim 4, low consumption active component wherein are selected from bensulfuron-methyl and chlorine sulphur is grand.
6. according to each described method among the claim 3-5, comprising the active component of 50wt% at least.
7. method according to claim 6, wherein at least 25% of active component dissolving after 5 ℃, 15 minutes in the composition.
8. method according to claim 7, wherein at least 40% of active component dissolving after 5 ℃, 5 minutes in the composition.
9. according to each described method among the claim 3-5, comprise the active component that is lower than 7wt%.
10. method according to claim 9, wherein at least 70% of active component dissolving after 5 ℃, 15 minutes in the composition.
11. method according to claim 10, wherein at least 70% of active component dissolving after 5 ℃, 5 minutes in the composition.
12. according to the described method of aforementioned arbitrary claim, alkaline, inorganic salts wherein comprises alkali metal salt.
13. method according to claim 12, alkali metal salt wherein comprises sodium carbonate.
14. according to the described method of aforementioned arbitrary claim, alkaline, inorganic salts wherein is anhydrous.
15. according to the described method of aforementioned arbitrary claim, active agricultural chemicals wherein is selected from bensulfuron-methyl and chlorine sulphur is grand, alkaline, inorganic salts comprises sodium carbonate.
16. method according to claim 15, active component wherein comprises i) bensulfuron-methyl and Stam F-34 or the ii) grand and isoproturon of chlorine sulphur.
17. according to the described method of aforementioned arbitrary claim, wherein in the composition weight ratio of total pesticide activity component and alkaline, inorganic salts for being no more than 10: 1, and at least 1: 3.
18., also comprise the dispersant that is selected from non-ionic surface active agent and anion surfactant according to the described method of aforementioned arbitrary claim.
19. method according to claim 18, dispersant are selected from the non-ionic surface active agent of the about 0mV of eletrokinetic potential and eletrokinetic potential surpasses-anion surfactant of 30mV.
20. one kind strengthens speed and the degree methods that pesticide activity component dissolves in water-bearing media, this method comprises that preparation contains the composition of pesticide activity component and alkaline, inorganic salts, so that 1% aqueous solution of said composition has at least 8 pH value when carrying out CIPAC Test MT75.3, with make composition by extruding the pre-composition that contains this active component and salt and optional dispersant, wherein before extruding, do not form paste.
21. alkaline, inorganic salts is the application in the composition pesticide as described in each in as claim 1-19, the ratio of active component dissolving in the composition when mixing with aqueous solution in order to increase, and improve plant or the on-site conveying that active component is handled to desire thus.
22. containing, application according to claim 21, composition wherein account for composition weight 10% active component at the most, and at least 70% after 5 ℃, 15 minutes, being dissolved in the CIPAC D water of the active component in the composition.
23. application according to claim 21, composition wherein contains the active component above composition weight 10%, and at least 25% being dissolved in after 5 ℃, 15 minutes in the CIPAC D water of the active agent in the composition.
24. composition that obtains by each described method among the claim 1-19, wherein said composition contains the active component that is at most composition weight 10%, the ratio that active component dissolves after 5 ℃, 15 minutes is at least 30%, above the dissolving ratio of active component in the comparative composition that replaces described salt with inert filler.
25. composition that obtains by each described method among the claim 1-19, wherein said composition contains the active agent that is at least composition weight 50%, the ratio that active component dissolves after 5 ℃, 15 minutes is at least 100%, above the dissolving ratio of active component in the comparative composition that replaces described salt with inert filler.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0413209.8 | 2004-06-14 | ||
| GB0413209A GB0413209D0 (en) | 2004-06-14 | 2004-06-14 | Chemical composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1988799A true CN1988799A (en) | 2007-06-27 |
Family
ID=32732444
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA200580024955XA Pending CN1988799A (en) | 2004-06-14 | 2005-06-14 | Process for producing a granular agrochemical composition |
Country Status (5)
| Country | Link |
|---|---|
| EP (1) | EP1773120A2 (en) |
| JP (1) | JP2008502643A (en) |
| CN (1) | CN1988799A (en) |
| GB (1) | GB0413209D0 (en) |
| WO (1) | WO2005120227A2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104853605A (en) * | 2012-12-12 | 2015-08-19 | 巴斯夫公司 | Solid agroformulations for preparing near micro-emulsion aqueous pesticides |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AR041211A1 (en) | 2002-09-12 | 2005-05-11 | Du Pont | PROCEDURE TO PREPARE SULFONAMIDE COMPOSITIONS EXTRUDED IN PASTA |
| AR081621A1 (en) * | 2010-02-04 | 2012-10-10 | Bayer Cropscience Ag | PROCEDURE FOR THE PRODUCTION OF STABLE FORMULATIONS OF SOLID SULFONAMID MATERIALS |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA1022848A (en) * | 1973-01-29 | 1977-12-20 | Imperial Chemical Industries Limited | Pesticidal compositions |
| AU558344B2 (en) * | 1983-04-04 | 1987-01-29 | E.I. Du Pont De Nemours And Company | Stabilized aqueuos solutions of sulphonylureas |
| CS253327B1 (en) * | 1986-04-01 | 1987-11-12 | Marie Vanova | Synergic herbicide |
| CA2054054C (en) * | 1990-10-31 | 2002-11-26 | Richard David Houghton | Propanil dispersible granule formulation |
| GB2298609A (en) * | 1995-02-28 | 1996-09-11 | Collag Manufacturing Limited | Apparatus for producing an extrudate |
| JP4084416B2 (en) * | 1995-12-01 | 2008-04-30 | バイエル・クロップサイエンス・アクチエンゲゼルシャフト | A stable mixture of incompatible active ingredients to protect plants |
| GB9901479D0 (en) * | 1999-01-22 | 1999-03-17 | Collag Ltd | Process for producing water soluble and water dispersible granules |
| GB9920281D0 (en) * | 1999-08-26 | 1999-10-27 | Collag Ltd | Novel compositions of biologically active agents and their use |
| AR041211A1 (en) * | 2002-09-12 | 2005-05-11 | Du Pont | PROCEDURE TO PREPARE SULFONAMIDE COMPOSITIONS EXTRUDED IN PASTA |
-
2004
- 2004-06-14 GB GB0413209A patent/GB0413209D0/en not_active Ceased
-
2005
- 2005-06-14 CN CNA200580024955XA patent/CN1988799A/en active Pending
- 2005-06-14 EP EP05755557A patent/EP1773120A2/en not_active Withdrawn
- 2005-06-14 WO PCT/EP2005/006860 patent/WO2005120227A2/en active Application Filing
- 2005-06-14 JP JP2007515904A patent/JP2008502643A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104853605A (en) * | 2012-12-12 | 2015-08-19 | 巴斯夫公司 | Solid agroformulations for preparing near micro-emulsion aqueous pesticides |
| US10390528B2 (en) | 2012-12-12 | 2019-08-27 | Basf Corporation | Solid agroformulations for preparing near micro-emulsion aqueous pesticides |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2005120227A3 (en) | 2006-03-30 |
| GB0413209D0 (en) | 2004-07-14 |
| WO2005120227A2 (en) | 2005-12-22 |
| EP1773120A2 (en) | 2007-04-18 |
| JP2008502643A (en) | 2008-01-31 |
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