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WO2017060349A1 - Capsules de cire creuses avec libération réduite en dioxyde de carbone pour attirer des parasites vivant dans le sol - Google Patents

Capsules de cire creuses avec libération réduite en dioxyde de carbone pour attirer des parasites vivant dans le sol Download PDF

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Publication number
WO2017060349A1
WO2017060349A1 PCT/EP2016/073874 EP2016073874W WO2017060349A1 WO 2017060349 A1 WO2017060349 A1 WO 2017060349A1 EP 2016073874 W EP2016073874 W EP 2016073874W WO 2017060349 A1 WO2017060349 A1 WO 2017060349A1
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WO
WIPO (PCT)
Prior art keywords
hollow
melt
gas
soil
stream
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
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PCT/EP2016/073874
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English (en)
Inventor
Christian Sowa
Max SIEBERT
Holger Kreusch
Ronald Wilhelm
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BASF SE
Original Assignee
BASF SE
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Filing date
Publication date
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Publication of WO2017060349A1 publication Critical patent/WO2017060349A1/fr
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Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01M—CATCHING, TRAPPING OR SCARING OF ANIMALS; APPARATUS FOR THE DESTRUCTION OF NOXIOUS ANIMALS OR NOXIOUS PLANTS
    • A01M1/00—Stationary means for catching or killing insects
    • A01M1/02—Stationary means for catching or killing insects with devices or substances, e.g. food, pheronones attracting the insects
    • A01M1/023—Attracting insects by the simulation of a living being, i.e. emission of carbon dioxide, heat, sound waves or vibrations
    • 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
    • A01N25/002—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 containing a foodstuff as carrier or diluent, i.e. baits
    • A01N25/006—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 containing a foodstuff as carrier or diluent, i.e. baits insecticidal
    • 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
    • A01N25/26—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 in coated particulate form

Definitions

  • the present invention relates to hollow wax capsules with reduced carbon dioxide release and to their preparation and use for attracting soil-dwelling pests.
  • CO2 carbon dioxide
  • the larvae of the Western corn rootworm and those of the black vine weevil exploit the CO2 concentration for localizing the roots of plants so as to subsequently exploit these roots as a food source. They reach the roots by moving along the CO2 gradient toward a higher CO2 concentration.
  • E.A. Bernklau et al. Journal of Economic Entomology 2004, 97, 330-339) describe a method for attracting pests in which particles comprising an organic substrate, baker's yeast and suitable nutrients, are employed from which CO2 is released.
  • the CO2 is formed and released by the yeast bacteria, which keeps the larvae of the Western corn rootworm away from the roots of corn plants.
  • WO 2014/041 1 12 A1 discloses particles for attracting soil-dwelling pests, made of a solid core comprising a nutrient such as starch and/or corn meal, a microorganism such as yeast, an insecticide and optionally further additives, and a solid shell of biodegradable biopolymers, and capsules which comprise these particles.
  • the release of the attractant CO2 is achieved by the microorganism metabolizing the nutrients, during which process the metabolite CO2 is excreted, among others.
  • suitable substances for the solid shell are the biodegradable biopolymers alginate, carrageenan, cellulose, hemicellulose, starch, chitin, chitosan, pectinate, guar gum, acacia gum, poly-D,L-lactic acid, gelatin, poly-amino acids, lignin and mixtures of these.
  • a disadvantage of the C02-releasing formulations or shaped articles described in the prior art is that CO2 is released in an uncontrolled fashion and/or too quickly, so that an effective CO2 gradient can only be maintained for a short period of time. To efficiently control the soil-dwelling pests, however, it is necessary to maintain the CO2 gradient over a prolonged period, preferably at least four weeks.
  • the object of the present invention is therefore to provide formulations or shaped articles which ensure such a delayed release of CO2 that a CO2 gradient which is efficient for controlling soil-dwelling pests is maintained over a prolonged period, preferably four or more weeks.
  • C02-comprising (hollow) capsules for controlling soil-dwelling pests and/or for reducing the yield loss caused by soil-dwelling pests has not been described to date.
  • C02-comprising capsules have not been mentioned to date in connection with the control of soil-dwelling pests.
  • C02-comprising (hollow) capsules have only been mentioned to date in a different connection.
  • WO 00/47042 A1 discloses C02-comprising capsules which comprise CO2 as a fish attractant. These capsules may be used as part of a bait for angling.
  • the fish attractants comprised in the capsules are composed of solid particles comprising a water-soluble meltable material as well as gas bubbles enclosed in the material, which gas bubbles consist fully or partially of CO2.
  • the capsules Upon contact with water, the capsules dissolve within a short time (preferably within 5 to 20 minutes), and the gas bubbles are released in an acoustically and visually discernible manner and rise to the water surface.
  • the fish are capable of perceiving the gas bubbles via their sense of vision and hearing, and are attracted thereby.
  • soil-dwelling pests such as, for example, various larvae of beetles from the family Elateridae, the Chrysomelidae and the Curculionidae may be controlled efficiently, i.e. lured away from the roots of the crop plants, over a prolonged period, preferably three or more weeks.
  • the larvae of these beetles feed in particular on the roots of crop plants such as potatoes, corn or strawberries. This is why the hollow capsules according to the invention are also suitable for reducing the yield losses in the production of potatoes, corn and
  • the hollow capsules according to the invention make it possible to maintain an efficient CO2 gradient within a certain radius around the hollow capsules over a prolonged period.
  • the C02-comprising gas (ki) therefore has a CO2 content of at least 20% by volume.
  • the expression "over a prolonged period” is understood as meaning that CO2 is released from the hollow capsule over a period of more than 2 weeks.
  • the CO2 concentration in the immediate vicinity of a hollow capsule is higher than in a region further away from the hollow capsule so that a CO2 gradient is established in the direction of the hollow capsule, in particular in the soil.
  • the capsule shell (S) of the hollow capsule is formed such that it completely encloses the hollow core (C), so that the C02-comprising gas (ki) cannot immediately escape fully from the hollow core (C).
  • the CO2 content in the C02-comprising gas (ki) amounts to between 40 and 100% by volume.
  • the C02-comprising gas (ki) especially preferably has a CO2 content of between 50 and 100% by volume and very especially preferably a CO2 content of between 70 and 100% by volume.
  • wax composition (hi)
  • Suitable waxes or types of waxes are in particular those which per se or together with other waxes or types of waxes have a melting point (TM) in the range of from 40 to 95°C in a composition.
  • TM melting point
  • the expression "wax” is understood as meaning any composition which has the following properties: - kneadable, solid to brittly hard at 20°C;
  • the wax composition (hi) may comprise natural, partly synthetic and/or synthetic waxes.
  • the natural waxes comprise, beside vegetable waxes and animal waxes, for example also petroleum waxes such as paraffin waxes.
  • Examples of synthetic waxes are polyolefins such as polyethylene.
  • the wax composition (hi) comprises one or more waxes which are selected from the group consisting of polyolefin waxes (hn) and petroleum waxes (hi2). Examples of such polyolefin waxes (hn) are substituted and unsubstituted
  • the wax composition (hi) preferably comprises a polyolefin wax (hn). If the wax composition (hi) comprises a polyolefin wax (hn), the latter preferably comprises one or more polyethylene compounds of the formula (I)
  • R 1 is selected independently from the group consisting of H, Ci-C4-alkyl, C1-C20- alkoxy and
  • p is an integer in the range from 10 to 70.
  • Ci-C4-alkyl comprises the hydrocarbon groups methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl and tert-butyl.
  • Ci-C2o-alkoxy comprises, within the scope of the present invention, the alkyloxy groups methoxy, ethoxy, n-propyloxy, isopropyloxy, n-butyloxy, sec-butyloxy, isobutyl, tert-butoxy, n-pentyloxy, 1 -methylbutyloxy, 2-methylbutyloxy, 3-methylbutyloxy, 1 ,1 -dimethylpropyloxy, 2,2-dimethylpropyloxy,
  • n-pentadecyloxy n-hexadecyloxy, n-heptadecyloxy, n-octadecyloxy, n-nonadecyloxy, n-eicosanyloxy, isononyloxy, isodecyloxy, isoundecyloxy, isododecyloxy,
  • R 1 is preferably selected from H, Me, n-hexadecyloxy, n-octadecyloxy and
  • Suitable polyolefin waxes are obtainable from a multitude of manufacturers (for example Luwax V from BASF SE).
  • the petroleum waxes (hi2) include, for example, macrocrystalline paraffin waxes and microcrystalline paraffin waxes.
  • wax composition (hi) comprises a petroleum wax (hi2)
  • the latter preferably comprises one or more paraffins of the formula (II)
  • R 2 represents H or methyl
  • m is an integer in the range from 15 to 40.
  • Suitable petroleum waxes are likewise commercially available.
  • a petroleum wax which is suitable is, for example, Sasolwax 5006 from BASF SE.
  • the wax composition (hi) comprises at least 30% by weight of the polyolefin wax (hn), based on the total weight of the wax composition (hi). In another preferred embodiment, the wax composition (hi) comprises at least 20% by weight of the petroleum wax (hi2), based on the total weight of the wax composition
  • the wax composition (hi) comprises at least 30% by weight of the polyolefin wax (hn) and at least 20% by weight of the petroleum wax (hi2), based on the total weight of the wax composition (hi).
  • the wax composition (hi) may additionally comprise further adjuvants whose purpose it is to influence the physical properties - such as, for example, the viscosity and/or the melting point - of the wax composition (hi) so as to thereby delay or accelerate the rate at which CO2 is released.
  • melting point is understood as meaning the melting point at atmospheric pressure (1013 hPa).
  • the hollow capsule according to the invention i.e. the capsule shell (S) has an external diameter (ds) in the range of from 1 .0 to 8.0 mm.
  • the external diameter (ds) of the capsule shell (S) is preferably in the range of from 2.0 to 8.0 mm, especially preferably in the range of from 2.0 to 6.0 mm.
  • the rate at which CO2 is released from the hollow capsules according to the invention may also be influenced via the wall thickness of the capsule shell (S).
  • the hollow core (C) of the hollow capsule preferably has a core diameter (dc) which amounts to between 20 and 95% of the external diameter (ds) of the capsule shell (S).
  • the capsule shell (S) of the hollow capsule accordingly, has a thickness (wall thickness) which amounts to between 3 and 40% of the external diameter (ds) of the capsule shell (S).
  • the core diameter (dc) especially preferably amounts to between 50 and 90%, very especially preferably between 70 and 90%, of the external diameter (ds) of the capsule shell (S).
  • the capsule shell (S) of the hollow capsules according to the invention may additionally comprise one or more additives ( i2).
  • the hollow capsules according to the invention may, for example, comprise further attractants, besides CO2, which attract the soil-dwelling pests. These attractants are in particular those which attract the soil- dwelling pests toward the hollow capsules over a shorter distance, optionally for them to be able to be killed optionally there.
  • the additive ( i2) is selected from the group consisting of feedants ( i2i) and pheromones ( i22).
  • Suitable feedants (h.21) and pheromones ( i22) are, in principle, known to a person skilled in the art.
  • a further aspect of the present application is the use of the hollow capsules according to the invention for attracting soil-dwelling pests, in particular larvae of beetles from the family Elateridae, the family Chrysomelidae and the family Curculionidae.
  • the hollow capsules according to the invention may be introduced between the placed seeds or plantlets.
  • the hollow capsules according to the invention can be introduced simultaneously with the seeds of the corresponding plant or the plantlets.
  • the hollow capsules according to the invention may be introduced at a later point in time.
  • the family Elateridae also comprises the subfamily Elaterinae, whose larvae are generally referred to as wireworms.
  • the larvae of a series of species from this subfamily are considered to be pests not only in agriculture, but also in forestry and in horticulture.
  • wireworms of the genus Agriotes whose members (Agriotes lineatus, A. obscurus, A. sputator, A. ustulatus and A. sordidus) are frequently referred to as click beetles, feed on the subterranean parts of virtually all crop plants and ornamentals. Corn, potatoes and beet are particularly affected. In vegetable growing, lettuces, lamb's lettuce, carrots and onions are especially susceptible to wireworm attack.
  • a further aspect of the present application is a method for reducing yield loss of useful plants, in particular potatoes, corn and strawberries, comprising the steps: (a) positioning the hollow capsules according to the invention in the immediate vicinity of the useful plants,
  • the capsule shell (S) of the hollow capsules according to the invention additionally comprises an insecticidal active substance (!3 ⁇ 4) so as to not only attract the soil-dwelling pests, but also to kill them.
  • an insecticidal active substance !3 ⁇ 4
  • Insecticidal active substances which are suitable for controlling, i.e. killing, the soil- dwelling pests, in particular larvae of beetles from the family Elateridae, the family Chrysomelidae and the family Curculionidae, are, in particular,
  • neonicotinoids/chloronicotinyl compounds such as imidacloprid, acetamiprid, nitenpyram, thiacloprid, thiamethoxam, terafuranitdine; pyrrols, such as
  • organophosphates such as acephate, azinphosmethyl, chlorpyrifos, dimethoate, disulfoton, fosthiazate, methamidophos, methidathion, methylparathion, oxydemetonmethyl, phorate, phosalone, phosmet, profenofos, trichlorfon, malathion, phosphamidon, monocrotophos, fenitrothion, diazinon, EPN; carbamates, such as alanycarbamate, aldicarbamate, benfuracarbamate, carbofurans, carbosulfans, furathiocarbamates, pirimicarbamates, thiodicarbamates,
  • fenobucarbamtes fenobucarbamtes
  • pyrethroids such as bifenthrin, cyfluthrin, cypermethrin,
  • the insecticidal active substance (!3 ⁇ 4) in the capsule shell (S) is preferably selected from the group consisting of imidacloprid, acetamiprid, nitenpyram, fipronil, carbofuran, carbosulfan, benfuracarb, thiacloprid, fludioxonil, nidinotefuran (MTI-446), thiamethoxam, clothionidin, terfuranitdine and mixtures of these.
  • the insecticidal active substance (!3 ⁇ 4) is especially preferably nidinotefuran (MTI-446), fipronil, thiacloprid, imidacloprid, clothionidin or a mixture of these.
  • An aspect of the present application is also the use of the hollow capsules according to the invention whose capsule shell (S) additionally comprises an insecticidal active substance (!3 ⁇ 4) for attracting and killing soil-dwelling pests, in particular larvae of beetles from the family Elateridae, the family Chrysomelidae and the family
  • the soil-dwelling pests which are attracted and killed are preferably wireworms (Elaterinae), larvae of the Western corn rootworm (Diabrotica virgifera) and/or larvae of the black vine weevil (Otiorhynchus sulcatus).
  • Subject matter of the present application is also a method of reducing the yield loss of useful plants, in particular potatoes, corn and strawberries, comprising the steps: (a) positioning the hollow capsules whose capsule shell (S) additionally comprises an insecticidal active substance (!3 ⁇ 4) according to the invention in the immediate vicinity of the useful plants,
  • a further aspect of the present application is a process for the preparation of the hollow capsules according to the invention, comprising the steps:
  • a capsule material comprising a wax composition (hi) and optionally one or more additives ( i2) and/or an insecticidal active substance (hs);
  • the capsule material (h), which comprises at least one wax composition (hi), is provided.
  • the capsule material (h2) and/or insecticidal active substances (!3 ⁇ 4) is preferably added as a finely divided solid.
  • the capsule material (h) is molten by increasing the temperature above the melting point (TM) of the wax composition (hi). Any solids particles which have not dissolved or molten at the selected processing temperature are dispersed in the melt.
  • the solids particles may take the form of, for example, an additive ( i2) or an insecticidal active substance (!3 ⁇ 4).
  • the melt (Oh) obtained preferably has a viscosity in the range of from 100 mPa-s to 1000 mPa-s, especially preferably a viscosity in the range of from 200 mPa-s to 800 mPa-s, very especially preferably a viscosity in the range of from 200 mPa-s to 400 mPa-s.
  • the density of the melt (Oh) is preferably less than 1 .0 g/cm 3 at the selected processing temperature.
  • the temperature and the residence time are chosen such that any insecticidal active substances (!3 ⁇ 4) which are present are not, or at least not
  • a stream of the melt (Oh) is generated.
  • this may be effected by introducing the melt (Oh) into a channel, through a nozzle.
  • the stream of the melt (Oh) is preferably passed through a channel with an internal cross-sectional diameter in the range of from 1 .0 to 10 mm.
  • process step b) a stream of gas (Gk) is passed into the stream of the melt (Oh) such that the stream of gas (Gk) is broken and individual gas bubbles are generated which are dispersed in the continuous phase of the stream of the melt (Oh) (cf. figures 1 a) to d)).
  • the stream of gas (Gk) no specific limitations exist, in principle, in respect of the selection of gases.
  • the only requirement is that the CO2 content in the CO2- comprising gas (ki) is at least 20% by volume.
  • the C02-comprising gas (ki) will, in addition to CO2, comprise for example air, oxygen, nitrogen and/or argon.
  • the stream of gas (Gk) is preferably passed through a channel with an internal cross- sectional diameter in the range of from 1 .0 to 8.0 mm.
  • the ratio of the volume streams between the stream of the melt (Oh) and the stream of gas (Gk) is, as a rule, between 10:1 and 1 :1 , preferably between 5:1 and 1 :1 .
  • Combining the stream of gas (Gk) and the stream of the melt (Oh) is carried out in a first dispersion zone. It is here that the melt stream comprising dispersed gas bubbles (Gk/Oh dispersion) is formed.
  • the first dispersion zone can be designed in various ways. By way of example, figure 1 shows three widespread designs of the first dispersion zone.
  • the first dispersion zone may be designed as a T-junction (see figure 1 a)).
  • the first dispersion zone in this case consists of two channels which are connected to each other in the shape of a T.
  • the horizontal channel (Mojn) conveys the stream of the melt (Oh) in the direction of the arrow towards the T-junction, while the channel (Mcin) introduces the stream of gas (Gk) perpendicular to the direction of the flow of the stream of the melt (Oh) into the T-junction.
  • the dimensions of the channels are chosen in such a way here that individual gas bubbles may form.
  • FIG. 1 b Another possible design of the first dispersion zone is shown diagrammatically in figure 1 b). It consists of a planar channel system which is characterized in that a horizontal channel crosses a channel which is perpendicular thereto, so that the channel system has three feed openings and one discharge opening. In this design, therefore, three streams are combined to one, which is therefore frequently referred to as a "flow-focusing device", or simply "flow focusing".
  • the horizontal channel (Mcin) conveys the stream of gas (Gk) in the direction of the arrow into the junction.
  • Streams of the melt (Oh) are conveyed, in the channels (Mojn) which are perpendicular to the direction of the flow of the stream of gas (Gk) in the direction of the arrow to the center of the junction, the stream of gas (Gk) being exposed to shear forces and breaking at the entry opening of the junction (diameter: dc/A,out, length: IG/A,OUI), and a melt stream comprising dispersed gas bubbles (Gk/Oh dispersion) originating in the horizontal channel (MG/A,OU , which melt stream exits from the stream-focusing device in the direction of the arrow.
  • the stream-focusing arrangement (figure 1 b)) not only two, but four parameters must be taken into consideration for isolated gas bubbles to be formed. Besides the parameters dcjn and dc/o.out which must be taken into
  • the first dispersion zone consists of an inner cylindrical channel and a coaxially arranged outer channel.
  • the stream of the melt (Oh) is conveyed in the direction of the arrow, while the stream of gas (Gk) is passed in via the inner channel in such a way that it breaks at the entry opening (dcin) and isolated gas bubbles form.
  • the diameters of entry opening (dcin) and discharge opening (cross- sectional diameter dG/o,out) are largely without effect on the formation of gas bubbles here.
  • the generation of the dispersed melt stream comprising gas bubbles is possible not only with the three described designs of the first dispersion zone, but can, of course, also be achieved with other designs.
  • the designs or channel arrangements described in the literature hereinbelow are also suitable: DE 10 2006 036 815 (A1 ), DE 10 2005 037 401 (B4).
  • the cross-sections of the channels, the viscosity of the melt (Oh) and the flow rates of the streams conveyed to the first dispersion zone are chosen such that the gas bubbles generated have the same diameter as the hollow core (C) of the hollow spheres according to the invention should later have, too.
  • step e) of the process the melt stream (Gk/Oh dispersion) is combined with an aqueous medium (A) in a second dispersion zone, where the melt stream (Gk/Oh dispersion) is cut off and individual dispersed melt drops, in each case enclosing one gas bubble, are formed in the aqueous medium (Gk/Oh/A dispersion).
  • the second dispersion zone may come in different designs.
  • the melt stream (Gk/Oh dispersion) may simply be passed into a container which is filled with the aqueous medium (A).
  • the dispersed melt stream comprising dispersed gas bubbles is passed into the aqueous medium (A) vertically from underneath.
  • the hollow capsules according to the invention - once the melt (Oh) has hardened in the aqueous medium (A) to give a solid capsule shell (S) - may simply be scooped up on the surface of the aqueous medium (A).
  • Another design of the second dispersion zone is shown diagrammatically in figure 2.
  • This design differs in particular in that the melt stream comprising dispersed gas bubbles (Gk/Oh dispersion) is combined here with a stream of the aqueous medium (A).
  • This design is identical in character with the possible design of the first dispersion zone, which has already been described hereinabove and shown in figure 1 b).
  • the melt stream (Gk/Oh dispersion) generated in process step d) is passed into the second dispersion zone in the direction of the arrow.
  • each stream of the aqueous medium (A) is passed into the second dispersion zone in the direction of the arrow.
  • the melt stream comprising dispersed gas bubbles (Gk/Oh dispersion) is then cut off such that individual melt drops form which, in turn, comprise in each case one enclosed gas bubble.
  • the stream of the aqueous medium which comprises dispersed melt drops (Gk/Oh/A dispersion) leaves the second dispersion zone in the direction of the arrow.
  • the dispersed melt drops, in each case enclosing one gas bubble are preferably fully or partially cooled in the aqueous medium (A), especially preferably while the melt drops, in each case enclosing one gas bubble rise in the aqueous medium (A).
  • the temperature of the aqueous medium (A) may be identical in all of the aqueous medium (A) or may differ locally.
  • the temperature of the aqueous medium (A) is higher at the point at which the melt stream (Gk/Oh dispersion) is passed in than at the point at which the hollow capsules according to the invention are isolated after having hardened at least partially.
  • the aqueous medium (A) may comprise further components; however, they are not required as a matter of principle. Depending on which viscosity and which density the melt (Oh) has, however, it may be advantageous to add a cosolvent and/or other additives to the aqueous medium (A).
  • the interfacial tension between the aqueous medium (A) and the melt (Oh) is generally between 20 and 80 mN-m, preferably between 25 and 60 mN-m, especially preferably between 30 and 60 mN-m.
  • interfacial tension refers to forces which arise between two different phases which are in contact with each other. The two phases form a joint interface which is under interfacial tension.
  • the dispersed melt drops in each case enclosing one gas bubble are cooled in the aqueous medium (A) to temperatures which are below the melting point of the (TM) of the wax composition (hi).
  • the melt (Oh) hardens and solid capsule shells (S) are formed.
  • the hollow capsules according to the invention can be isolated in a simple manner after the capsule shells (S) have fully or at least partially hardened.
  • Figure 1 shows various designs of the first dispersion zone in which the melt stream comprising dispersed gas bubbles (Gk/Oh dispersion) can be formed;
  • figure 1 a) is a diagrammatic representation of the formation of a dispersion in a T-junction;
  • figure 1 b) is a diagrammatic representation of the formation of monodispersed gas bubbles in a flow-focusing device;
  • figure 1 c) is a diagrammatic representation of the formation of a dispersion in a device consisting of coaxial channels.
  • Figure 2 shows a design of the second dispersion zone in which a stream of dispersed melt drops, in each case enclosing one gas bubble, can be formed in aqueous medium (Gk/Oh/A dispersion).
  • a stream of dispersed melt drops in each case enclosing one gas bubble, can be formed in aqueous medium (Gk/Oh/A dispersion).
  • Gk/Oh/A dispersion aqueous medium
  • Luwax V and Sasolwax 5006 (melting point (TM): 53°C), to 80% of the capacity.
  • Tube connections were made with PTFE tubes (external diameter 1 .6 mm, internal diameter 1 .0 mm). Then, the cartridge was attached to the hydraulic wax conveyance on the entry side, via the Swagelok screw joint, and to the gas capsule formation unit on the opposite discharge side, likewise via a Swagelok screw joint.
  • the cartridge filled with the wax composition (hi) was hung vertically into a water bath so that the discharge side points upward. Then, the water bath was warmed to 65°C, thereby melting the wax composition (hi).
  • the hydraulic conveying unit at the entry side consists of a stainless-steel pressure vessel, arranged upstream, from Sartorius, filled with water and connected to 3 bar pressurized air, and, arranged downstream, a volume flow control consisting of a Coriflow M12C2 control unit (Bronkhorst), which works on the basis of the Coriolis principle, and from there into the wax cartridge.
  • the stream of gas (Gk) is passed in through the second limb of the Y-shaped piece. Then, wax and gas together flow toward the discharge opening which is adapted, by means of an adapter at the bottom, into an upward glass tube.
  • the fluid in the hardening and collecting basin for the manufactured hollow capsules is in the water (however, one may, for example, also carry out the process with additives in the water bath.
  • the density in the water bath may be adjusted by adding dissolved sodium chloride such that the detachment of the gas bubbles is supported.
  • the stream of the melt (O h ) was first adjusted to a volume flow of 35 ml/min, and the stream of gas (Gk) was
  • a stable melt stream comprising dispersed gas bubbles (Gk/Oh dispersion) could be observed.
  • Gk/Oh dispersion dispersed gas bubbles
  • the gas bubbles are discharged, uniformly and one after the other, from the discharge opening, become detached in the aqueous medium (A) of the water bath, rise up into the cooler temperature zone of the water bath, during which process they already harden to some degree, and float float into a connected collecting funnel for further hardening. From there, they are optionally skimmed off, dried and stored.
  • the hollow capsules obtained have an external diameter (ds) of between 4 and 6 mm. They are closed to a degree of more than 90% and reveal capsule-wall thicknesses of between 20 and 150 ⁇ when viewed under the light-optical microscope.
  • melt - Luwax V (50% by weight; poly(n-octadecyloxyethylene) with an averaged molar mass of 28 000 g/mol, melting point: 47-51 °C)
  • the release of CO2 from the hollow capsules is detected in the following laboratory experiment.
  • a laboratory flask 250 ml, Schott
  • the flask was closed by means of a screw cap (GL 45).
  • a CO2 sensor Almeno FYAD 00 CO2B10 (measuring range: 0 to 10 000 ppm CO2) for use in a universal measuring instrument Almeno 2590 (by Ahlhorn) and a plastic cannula were able to be inserted into the flask by means of specifically made openings in the screw cap.
  • Almeno 2590 by Ahlhorn
  • a plastic cannula were able to be inserted into the flask by means of specifically made openings in the screw cap.
  • the flask had been flushed with nitrogen until the measured CO2 concentration was stably at "0 ppm".

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  • Life Sciences & Earth Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Plant Pathology (AREA)
  • Toxicology (AREA)
  • Insects & Arthropods (AREA)
  • Dentistry (AREA)
  • Food Science & Technology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

La présente invention concerne une capsule creuse dotée d'une enveloppe de capsule solide (S) et d'un noyau creux (C), l'enveloppe de capsule (S) comprenant une composition de cire (h1) et le noyau (C) comprenant un gaz contenant du CO2 (k1), le gaz contenant du CO2 (k1) ayant une teneur en CO2 d'au moins 20 % en volume.
PCT/EP2016/073874 2015-10-07 2016-10-06 Capsules de cire creuses avec libération réduite en dioxyde de carbone pour attirer des parasites vivant dans le sol Ceased WO2017060349A1 (fr)

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EP15188788.2 2015-10-07

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10701937B2 (en) 2015-02-11 2020-07-07 Basf Se Pesticidal mixture comprising a pyrazole compound, an insecticide and a fungicide

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10701937B2 (en) 2015-02-11 2020-07-07 Basf Se Pesticidal mixture comprising a pyrazole compound, an insecticide and a fungicide

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