KR20140079483A - Stable formulations containing fumed aluminum oxide - Google Patents

Stable formulations containing fumed aluminum oxide Download PDF

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KR20140079483A
KR20140079483A KR1020147013034A KR20147013034A KR20140079483A KR 20140079483 A KR20140079483 A KR 20140079483A KR 1020147013034 A KR1020147013034 A KR 1020147013034A KR 20147013034 A KR20147013034 A KR 20147013034A KR 20140079483 A KR20140079483 A KR 20140079483A
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atrazine
methyl
suspension concentrate
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KR101931846B1 (en
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티모시 마틴
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에프엠씨 코포레이션
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/661,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
    • A01N43/681,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
    • A01N43/70Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

Abstract

The present invention provides a novel herbicidal aqueous solution or suspension concentrate composition comprising a herbicidally active agent with excellent chemical and physical stability as well as excellent redispersibility characteristics and a fumed alumina as a stabilizer.

Description

STABLE FORMULATIONS CONTAINING FUMED ALUMINUM OXIDE [0002]

The present invention relates to the field of agrochemical formulations.

In order to be able to effectively remove or control unwanted plants, it is desirable to use effective chemical agents of herbicides. Compositions comprising two or more herbicides are desirable in certain agricultural areas and related efforts since they extend the spectrum or range of unwanted plant species that are killed or controlled.

Since it is desirable to have a composition having the above-mentioned characteristics, it is useful to use a combination of herbicides that promote the control of multiple weeds by applying a single herbicide. Combinations of insecticides are known and are available as a mixed solution of the active ingredients in their commercially available preparations. One method of making such compositions is referred to as "tank mixing ", wherein the components of their commercially available form are mixed by a user with a quantity of water. Tank mixes require end-users to purchase more than one commercial product, store them, calculate the exact amount of each active ingredient, meter these quantities into a mix, and dispose of multiple containers as appropriate. Tank mixing of two or three different commercial formulations often results in physical instability causing precipitation, aggregation, phase separation, etc. of the active ingredients, thus providing a non-uniform distribution of active ingredients. While it is advantageous to combine the active ingredients into one formulation, it is often more complicated due to the very different physical properties of the active ingredients, where chemical and physical stability is a problem.

The present invention provides a novel herbicidal aqueous suspoemulsion or aqueous suspension concentrate composition comprising a fumed alumina as a herbicidal and stabilizing agent with excellent chemical and physical stability as well as excellent redispersion properties do.

The present invention provides a novel herbicidal water-in-vivo suspension emulsion or aqueous suspension concentrate composition comprising a herbicidally active and a fumed alumina as a stabilizer, with excellent re-dispersing properties as well as excellent chemical and physical stability.

In one embodiment, the present invention is directed to a herbicide comprising atrazine, pyroxasulfone and fluthiacet-methyl, which have excellent chemical and physical stability as well as excellent redispersion characteristics To a novel aqueous suspoic emulsion composition.

Specifically, the aqueous suspoic emulsion compositions of the present invention comprise:

i) an aqueous suspension concentrate composition comprising piroxysulfone and atrazine;

ii) an aqueous emulsion composition comprising fluthiacet-methyl; And

iii) Fumed alumina.

Another embodiment of the present invention is a compound of formula

i) forming an aqueous suspension concentrate composition comprising a piroxysulfone and atrazine;

ii) forming an aqueous emulsion composition comprising fluthiacet-methyl;

iii) blending together the suspension concentrate and the aqueous emulsion composition, and

iv) adding fumed alumina and blending the mixture to form a homogeneous mixture.

Another embodiment of the present invention is a compound of formula

i) forming an aqueous suspension concentrate composition comprising a piroxysulfone, atrazine and fumed alumina;

ii) forming an aqueous emulsion composition comprising fluthiacet-methyl;

iii) blending the suspension concentrate and the emulsion composition in water together to form a homogeneous mixture.

Another embodiment of the present invention is a compound of formula

i) an agriculturally active component comprising fluthiacet-methyl, atrazine and piroxysulfone;

ii) a surfactant component comprising an acrylic graft copolymer and a polyalkylene oxide block copolymer;

iii) defoamer;

iv) biocides;

v) pH adjusting agents;

vi) cryoprotectants; And

vii) an aqueous suspension concentrate composition comprising fumed alumina.

It has surprisingly been found that the addition of fumed alumina to a waxy emulsion or suspension concentrate composition provides unexpected physical and chemical stability to the composition. Other stabilizers, such as fumed silica, provide good chemical stability but lack physical stability when used in the susto emulsion or suspension concentrate composition of the present invention (for example, after 24 hours a precipitate forms at room temperature , Difficult to redistribute). The fumed alumina is added to the present sulfur emulsion or suspension concentrate composition to provide a chemically and physically stable composition. In the preparation of the suspension-emulsion composition, the fumed alumina can be added to the suspension concentrate composition portion or added to the final formulation composition; Preferably it is added to the suspension concentrate portion of the composition.

In one embodiment of the invention, the spore emulsion composition is formed by combining the suspension concentrate composition with an aqueous emulsion composition. Suspended concentrate (SC) is a preparation in which the solid active component (s) are suspended in a liquid carrier. The aqueous suspension concentrate composition portion of the Scoop Emulsion further comprises a surfactant component, a pH adjuster (optional), a cryoprotectant, a defoamer, and an antimicrobial (biocidal) formulation. Atrazine is present in an amount of from 40% to 55% by weight, preferably from 44% to 51% by weight, of all components in the SC composition. The pyrochlore phon is present in an amount of 5 wt% to 7 wt% of all components in the SC composition. The surfactant component is composed of two or more surfactants; Alkyl EO / PO copolymers and acrylic graft copolymers. The alkyl EO / PO copolymer is preferably a TERGITOL XD surfactant, available, for example, from Dow Chemicals and is present in an amount ranging from 2% to 3% by weight of all components in the SC composition % ≪ / RTI > The acrylic graft copolymer is preferably a TERSPERSE 占 2500 dispersant, available, for example, from Huntsman Performance Products, containing 3 wt% to 4 wt% of all components in the SC composition, ≪ / RTI > The pH adjusting agent is preferably an acid, for example glacial acetic acid, and is present in an amount of 0 to 0.13% by weight of all components in the SC composition. The cryoprotectant is preferably propylene glycol and is present in an amount of 5 wt% to 10 wt%, preferably 6 wt%, of all components in the SC composition. The antifoaming agent is preferably a silicone emulsion and is, for example, a DOWCORNING 占 AF emulsion, available from the Dow Chemical Company, containing from 0.05% to 0.5% by weight of all components in the SC composition, By weight, preferably 0.1% by weight. The biocide is preferably selected from the group consisting of, for example, KATHON (registered trademark) CG or LEGEND (registered trademark) MK from Dow Chemical Company, or Thor Specialties, Inc ) And is present in an amount of 0.05 wt.% To 0.5 wt.%, Preferably 0.1 wt.% Of all components in the SC composition. The stabilizing component is preferably a fumed alumina as the acidic aqueous dispersion, for example AERODISP (R) W 630 available from Evonik Industries, and all components in the SC composition And is present in an amount of from 0.5% to 2% by weight. The SC composition comprises a thickener, for example, magnesium aluminum silicate [ (Veegum: < / RTI > magnesium aluminum silicate from RT Vanderbilt Company).

An aqueous emulsion (EW) is a preparation in which droplets of a water-insoluble phase (oil or water-insoluble solvent) are uniformly distributed in water. The EW portion of the present susto-emulsion composition further comprises a water insoluble solvent, a surfactant component, a pH adjusting agent, a cryoprotectant, a defoamer and an antimicrobial agent (biocide). The fluticaset-methyl is present in an amount of 1 wt% to 2 wt% of all components in the EW composition. The solvent is preferably an aromatic solvent such as Aromatic 200 or Aromatic 200 ND available from ExxonMobil < (R) > Chemicals, from 45% to 50% of all components in the EW composition By weight. The surfactant component is composed of two or more surfactants; Nonionic polymeric surfactants and polyalkylene oxide block copolymers. The nonionic polymeric surfactant is preferably Atlox 4914, available from Crodia Crop Care, for example, from 4 wt% to 5 wt% of all components in the EW composition % ≪ / RTI > The polyalkylene oxide block copolymer is preferably, for example, Atlas (R) G-5000 available from Crodia Crop Care, and contains 4.5 wt.% To 5.5 wt.% Of all components in the EW composition Lt; / RTI > The pH adjusting agent is preferably an acid, for example glacial acetic acid, and is present in an amount of 0.01% to 0.1% by weight of all components in the EW composition. The cryoprotectant is preferably propylene glycol and is present in an amount of 5% to 10% by weight, preferably 6% by weight, of all components in the EW composition. The defoamer is preferably a silicone emulsion, for example a Dow Corning (registered trademark) AF emulsion available from Dow Chemical Company, containing from 0.05% to 0.5%, preferably 0.1% by weight of all components in the EW composition Lt; / RTI > The biocide is preferably, for example, Cartith (R) CG or Legic (R) MK from Dow Chemical Company or Actide (TM) MV from Tor Specialty Chemicals , And 0.05 wt% to 0.1 wt% of all components in the EW composition.

In another embodiment of the present invention, an aqueous suspension concentrate is formed using fumed alumina as the stabilizer. The aqueous suspension concentrate composition comprises an active ingredient comprising fluthiacet-methyl, pyroxysulfone and atrazine; A surfactant component comprising an acrylic graft copolymer and a polyalkylene oxide copolymer; Defoamer; Biocides; pH adjusting agents; Antifreeze agents; And stabilizers. The fluticaset-methyl is present in an amount of 0.1% to 0.2% by weight of all components in the SC composition. The pyroxenes are present in an amount of 5% to 7% by weight of all components in the SC composition. Atrazine is present in an amount of from 40% to 45% by weight of all components in the SC composition. The surfactant component is composed of an acrylic graft copolymer and a polyalkylene oxide block copolymer. The acrylic graft copolymer is preferably a Terps (R) 2500 dispersant, available, for example, from Huntsman Performance Products, and is present in an amount of 2.5% to 3.0% by weight of all components in the SC composition. The polyalkylene oxide block copolymer is preferably, for example, Atlas G-5000 available from Crodia Crop Care, and is present in an amount of from 2.5% to 2.75% by weight of all components in the SC composition do. The pH adjusting agent is preferably an acid, for example glacial acetic acid, and is present in an amount of 0.01% to 0.1% by weight of all ingredients in the SC composition. The cryoprotectant is preferably propylene glycol and is present in an amount of 5 wt% to 10 wt%, preferably 5.5 wt% to 6 wt% of all components in the SC composition. The defoamer is preferably a silicone emulsion, for example a Dow Corning (registered trademark) AF emulsion, available from Dow Chemical Company, and is present in an amount of 0.05% to 0.1% by weight of all components in the SC composition. The biocide is preferably selected from, for example, Carton (registered trademark CG) or Legend (registered trademark) MK from Dow Chemical Company, or Actide (registered trademark) MV from Tor Specialty Chemicals And is present in an amount of 0.01% to 0.1% by weight of all components in the total composition. The stabilizing component is preferably a fumed alumina as an acidic aqueous dispersion, for example Aerodisup (R) W 630, available from Ebonic Industries, and is present in an amount ranging from 0.5% to 2% by weight % ≪ / RTI >

The weight ratio of fluthiacet-methyl to pyroxhosphone to atrazine can vary widely, but is generally in the range of 1: 33: 284 to 1: 40: 325.

Certain embodiments of the present invention are methods for controlling unwanted plants, comprising applying an insecticidally effective amount of a composition of the present invention to an area where an unwanted plant is required to be controlled.

As used herein, unless otherwise indicated, the term "insecticide" refers to an undesirable plant, such as, but not limited to, an organism that inhibits or kills harmful or annoying weeds, light plants, grasses and sedges Refers to a molecule or combination of molecules that can be used for crop protection, building protection, and grass protection. The term "herbicidal amount" refers to an amount of a herbicide that is capable of eliminating, destroying, or running an observable herbicidal effect on unwanted plant growth, such as unwanted plant necrosis, killing, growth inhibition, reproductive inhibition, proliferation inhibition, Means the amount needed to represent the effect.

As used herein, the terms "ambient temperature" and "room temperature" refer generally to any suitable temperature found in the laboratory or other workplace, and generally below about 15 ° C or above 30 ° C.

As used herein, "weight percent of ingredients in the composition" includes weight percentages of all liquid and solid ingredients in the composition.

The methods and compositions of the present invention are further exemplified by the following examples. The embodiments are merely illustrative of the invention and should not be construed as limiting, as further modifications of the disclosed invention will be apparent to those skilled in the art. All such modifications are contemplated as falling within the scope of the invention as defined in the claims.

Example 1

Preparation of a sphero-emulsion concentrate formulation of atrazine, pyroxysulfone and fluthiacet-methyl using fumaric alunima as the stabilizer

Step A: Preparation of atrazine / pyroxysulfone suspension concentrate (SC)

17.0.90 grams of deionized water, 0.10 grams of glacial acetic acid, 36.00 grams of polyethylene glycol, 0.60 grams of defoamer (Dow TM Antifoam AF from Dow Chemical Company), 0.60 grams of preservative [from The Dow Chemical Company 14.10 grams of an alkyl EO / PO copolymer nonionic surfactant (Tergitol (registered trademark) XD from The Dow Chemical Company), 20.10 grams of an acrylic graft copolymer surfactant [ G-2500 available from Huntsman Performance Products), 7.80 grams of an aqueous dispersion of fumed alumina (Aerodisp @ W 630 from Ebonic Industries), 37.50 grams (99.3% purity) and 303.0 grams of atrazine (97.0% purity) was added to a 1 liter beaker and blended for 5 minutes at 4500 rpm with a Silverson homogenizer. The mixture was transferred to an Eiger grinder and milled at 3000 rpm for 15 minutes to achieve a particle size of D90 < 3 mu m.

Step B: Fluticaset-methyl water emulsion (EW)

12.36 grams (99.1% purity) of fluticaset-methyl and 47.50 grams of a nonionic polymeric surfactant (Atlox.RTM. 4914 from Crodia Crop Care) were dissolved in 475.00 grams of aromatic naphthalene depleted solvent Aromatic 200 ND from Mobil Chemicals). The mixture was stirred and heated to 65 DEG C to form a solution. This solution was added to 353.00 grams of deionized water with 0.50 grams of glacial acetic acid, 60.00 grams of propylene glycol, 50.00 grams of a polyalkylene oxide block copolymer (Atlas G5000 from Crodia Crop Care), 0.50 grams of defoamer [ Dow (TM) Antifoam AF from The Dow Chemical Company] and 1.00 grams of preservative (Carton (R) CG / ICP from The Dow Chemical Company). This mixture was homogenized by a Silverton homogenizer until a homogeneous mixture was formed.

Step C: Formation of a wastewater emulsion concentrate (SE)

A sarcoplasmic concentrate was formed by combining 367.82 grams of atrazine / piroxysulfone SC from Step A with 51.84 grams of fluthiacet-methyl EW from Step B and 4.67 grams of deionized water. The resulting composition was stirred until a homogeneous mixture was obtained. The resulting wastewater emulsion concentrate composition was uniformly dispensed into 8 oz glass bottles, sealed, and stored for 2 weeks at an elevated temperature of 54 캜 for stability testing. Analysis by High Performance Liquid Chromatography (HPLC) showed that after two weeks at elevated temperature: Initial analysis - Atrazine 42.33%; 5.35% of the Pirox private phone; 0.1% fluthiacet-methyl; Elevated temperature - atrazine 42.48%; 5.4% of the Pirox private phone; 0.1% fluthiacet-methyl; The composition was found to be chemically stable.

Visual inspection of the Sauvo emulsion concentrate composition at 2 weeks showed no phase separation or sedimentation, indicating that the composition is physically stable.

Example  2

Production of atrazine / pyroxysulfone suspension concentrate (SC) and fluticaset-methyl emulsion (EW) using fumed aluniima as stabilizers

In a similar manner to Example 1, Step A, additional SC compositions were prepared comprising atrazine and pyroxysulfone. In a similar manner to Example 1, Step B, additional EW compositions comprising fluthiacet-methyl were prepared. Additional SC compositions are summarized in Table 2A below; Table 2B summarizes additional EW compositions.

[Table 2A]

Figure pct00001

[Table 2B]

Figure pct00002

Example  3

Preparation of a sphero-emulsion concentrate formulation of atrazine, pyroxysulfone and fluthiacet-methyl using fumaric alunima as the stabilizer

Step A: Preparation of atrazine / pyroxysulfone suspension concentrate (SC)

2.3 grams of deionized water, 7.7 grams of glacial acetic acid, 463.0 grams of polyethylene glycol, 7.7 grams of antifoaming agent (Dow TM Antifoam AF from The Dow Chemical Company), 6.9 grams of preservative (Thorpe Specialty Chemicals Inc. 181.4 grams of an alkyl EO / PO copolymer nonionic surfactant (Tergitol (registered trademark) XD from The Dow Chemical Company), 258.5 grams of an acrylic graft copolymer interface The mixture of the active agent (Terpspus (R) G-2500 from Huntsman Performance Products) was added to the slurry tank and mixed until homogeneous. (480.0 grams, 99.3% purity) and atrazine (3.862.0 kg, 97.0% purity) were added in portions to the tank such that each addition was thoroughly mixed before the next portion was added. The mixture was transferred to a grinding mill, milled and maintained at a temperature below 30 DEG C until a particle size of D90 < 3 mu m was obtained. The ground mixture was transferred to a blending tank and 138.9 grams of an aqueous dispersion of fumed alumina (Aerodisp (registered trademark) W 630 from Ebonic Industries) was added. The mixture was stirred for 1 hour to give 6.79 kilograms of suspension concentrate.

Step B: Fluticaset-methyl water emulsion (EW)

141.4 grams of flutiacet-methyl (99.1% purity) and 544.5 grams of a nonionic polymeric surfactant (Atlox.RTM. 4914 from Crodia Crop Care) were mixed with 5.4446 kilograms of aromatic naphthalene decolouring solvent (ExxonMobil Chemical Aromatic &lt; / RTI &gt; 200 ND from Sigma) to produce an organic phase. The mixture was stirred in an in-line homogenizer in a 15 liter jacketed vessel and heated to 55 DEG C to form a solution. 5.7 grams of glacial acetic acid, 687.7 grams of propylene glycol, 573.1 grams of a polyalkylene oxide block copolymer (Atlas G5000 from Crodia Crop Care), 5.70 grams of defoamer (Dow from Dow Chemical Company &Lt; RTI ID = 0.0 &gt; Antifoam AF) &lt; / RTI &gt; and 4.0492 kilograms of deionized water to a mixing vessel and heated to 55 DEG C until a homogeneous mixture was obtained. The warm organic phase was added to the aqueous phase via the recycle line of the in-line homogenizer. Once the addition was complete, the homogenization was continued until a particle size of less than 3 microns was achieved in D90. The mixture was cooled to room temperature and 10.3 grams of preservative (Actideide (TM) MV from Torres Specialty Inc.) was added and stirred until approximately 11.2 kilograms of a homogeneous mixture was obtained.

Step C: Suhsoo emulsion concentrate (SE) formulation

6.658 kilograms of atrazine / piroxysulfone SC from step A were combined with 941.0 grams of fluthiacet-methyl EW from step B and 186.0 grams of deionized water to form a spore emulsion concentrate. The resulting composition was stirred until 7.77 kilograms of a homogeneous mixture was obtained. This suspension emulsion was stored in a separate sealed glass container.

Reference Example A

Preparation of a formulation of a waxy emulsion concentrate of atrazine, pyroxysulfone and fluthiacet-methyl using fumed silica as stabilizer

Step A: Preparation of atrazine / pyroxysulfone suspension concentrate (SC)

0.50 grams of de-ionized water, 0.50 grams of glacial acetic acid, 30.00 grams of polyethylene glycol, 0.50 grams of defoamer (Dow TM Antifoam AF from The Dow Chemical Company), 0.75 grams of preservative [from The Dow Chemical Company (Carton (R) CG / ICP), 11.75 grams of an alkyl EO / PO copolymer nonionic surfactant (Tergitol (R) XD from The Dow Chemical Company), 16.75 grams of an acrylic graft copolymer surfactant (Terus Spur (TM) G-2500 from Huntsman Performance Products), 2.50 grams of an aqueous dispersion of fumed silica (Aerodisp (R) W 7512 from Econonic Industries, a commonly used emulsion stabilizer S], a mixture of 25.75 grams of the Pirox private phone (99.3% purity) and 222.50 grams of atrazine (97.0% purity) was added to a 1 liter beaker and stirred for 5 minutes at 4500 rpm, It was blended in by. The mixture was transferred to an Eiger mill and milled at 3000 rpm for 15 minutes to achieve a particle size of D90 < 3 [mu] m.

Step B: Fluticaset-methyl water emulsion (EW)

18.54 grams (99.1% purity) and 71.25 grams of a nonionic polymeric surfactant (Atlox.RTM. 4914 from Crodia CropCare) were dissolved in 712.50 grams of an aromatic naphthalene decolouring solvent (ExxonMobil Chemical Aromatic &lt; / RTI &gt; 200 ND from &lt; RTI ID = The mixture was stirred and heated to 65 DEG C to form a solution. This solution was added to a solution of 0.75 grams of glacial acetic acid, 90.00 grams of propylene glycol, 75.00 grams of a polyalkylene oxide block copolymer (Atlas G5000 from Crodia CropCare), 0.75 grams of defoamer [ Dow (TM) Antifoam AF from Dow Chemical Company] and 2.25 grams of preservative (Carton (R) CG / ICP from The Dow Chemical Company). This mixture was homogenized by a Silverton homogenizer until a homogeneous mixture was formed.

Step C: Formation of a wastewater emulsion concentrate (SE)

449.3 grams of atrazine / piroxysulfone SC from Step A was combined with 50.8 grams of fluthiacet-methyl EW from Step B and 4.67 grams of deionized water to form a spore emulsion concentrate. The resulting composition was stirred until a homogeneous mixture was obtained. This suspension emulsion was stored in a separate sealed glass container.

Example 4

Preparation of aqueous suspension concentrates of atrazine, pyroxysulfone and fluthiacet-methyl using fumaric alunima as stabilizers

308.72 grams of deionized water, 0.72 grams of glacial acetic acid, 46.88 grams of polyethylene glycol, 0.72 grams of antifoaming agent (Dow TM Antifoam AF from The Dow Chemical Company), 0.72 grams of preservative (available from Thorpe Enterprises Incorporated 22.96 grams of an acryl-based graft copolymer surfactant (Terpers (TM) G-2500 available from Huntsman Performance Products, Inc.), 20.88 grams of a polyalkylene oxide block copolymer (Atlas G5000 from Crodia Crop Care), 12.32 grams of an aqueous dispersion of fumed silica (Aerodisup.RTM. W 7512 S from Ebonic Industries, a commonly used emulsion stabilizer) A mixture of 42.56 grams of Pyroxanese Phon (99.3% purity), 342.40 grams of atrazine (97.0% purity) and 1.20 grams of flutiaceet-methyl (99.1% Were added to the beaker and blended by Silverton homogenizer at 4500 rpm for 5 minutes. The mixture was transferred to an Eiger mill and ground until a particle size of D90 < 3 [mu] m was achieved. These SC preparations were stored in separate sealed glass containers.

Example 5

Physical and chemical stability data

(1%) or 3.0 grams (3%) from Example 3 and Reference Example A added to 99.0 ml or 97.0 ml of water having a hardness of 20 ppm or 500 ppm in a 100 ml Nessler tube. A dilute material dispersion study was conducted using a spoemic emulsion concentrate composition. The Nestler tube was sealed with a rubber stopper, and the contents were mixed by inverting the tube 10 times below. The resulting test sample was maintained at ambient temperature. Reproducibility of formulation The formulation was run for 24 hours and the number of reversals required to produce a homogeneous mixture was recorded. Table 4A below summarizes the redistributed data.

[Table 4A]

The resampling data from Example 3 and Reference Example A

Figure pct00003

The Sauvo emulsion concentrate compositions of Example 3 and Example 4 were tested for physical and chemical stability at 24 hours (initial), in a freeze / thaw cycle (at -30 ° C for 2 days / room temperature) Three days in two days), and 54 [deg.] C for two weeks. The waxy emulsion of Example 3 was also analyzed for physical and chemical stability at 50 占 폚 for 1 month and 3 months and at room temperature for 1 month. The sample viscosity (centipoise) was measured using a Brookfield RVT viscometer (spindle speed of spindle number 3, 50). The particle size was measured in D90 (90% of the particles were reported in microns) using a particle size distribution analyzer (Horiba Particle Scattering Particle Size Distribution Analyzer LA-910) . The separation rate (%) was visually determined by measuring the height of the separated layer and dividing the number by the total height of the container. Analysis of active ingredients was performed by HPLC analysis on a weight percent basis. These data are summarized in Table 4B below.

[Table 4B]

Figure pct00004

As can be seen from the data provided above, the physically and chemically stable compositions can be prepared by mixing the fumed alumina with an agricultural composition, such as a sulfo-emulsion preparation and a suspending agent, in comparison with a similar composition using a commonly used stabilizer such as fumed silica Concentrate formulation.

While the invention has been described with emphasis on preferred embodiments, it will be apparent to those skilled in the art that changes in the preferred apparatus and method may be employed and that the invention may be practiced otherwise than specifically described herein. Accordingly, the invention also includes all modifications embraced within the spirit and scope of the invention as defined by the following claims.

Claims (7)

i) an aqueous suspension concentrate composition comprising pyroxasulfone and atrazine;
ii) an aqueous emulsion composition comprising fluthiacet-methyl; And
iii) a suspoemulsion concentrate composition comprising fumed alumina.
The method according to claim 1,
Wherein the aqueous suspension concentrate further comprises at least one selected from the group consisting of a surfactant component, a pH adjuster, a cryoprotectant, a defoamer, a thickener, and an antimicrobial agent.
The method according to claim 1,
Wherein the aqueous emulsion concentrate further comprises at least one selected from the group consisting of a surfactant component, a pH adjuster, a cryoprotectant, a defoamer, a thickener, and an antimicrobial agent.
The method according to claim 1,
Wherein the weight ratio of fluthiacet-methyl to pyroxhosphone to atrazine is 1: 33: 284 to 1: 40: 325.
i) forming an aqueous suspension concentrate composition comprising a piroxysulfone and atrazine;
ii) forming an aqueous emulsion composition comprising fluthiacet-methyl;
iii) blending together the suspension concentrate and the aqueous emulsion composition, and
iv) adding fumed alumina and blending the mixture to form a homogeneous mixture.
i) forming an aqueous suspension concentrate composition comprising a piroxic and atrazine, and a fumed alumina;
ii) forming an aqueous emulsion composition comprising fluthiacet-methyl;
iii) blending the suspension concentrate and the aqueous emulsion composition together to form a homogeneous mixture.
i) agricultural active ingredients comprising fluthiacet-methyl, atrazine and pyroxysulfone;
ii) a surfactant component comprising an acrylic graft copolymer and a polyalkylene oxide block copolymer;
iii) defoamer;
iv) biocides;
v) pH adjusting agents;
vi) cryoprotectants; And
vii) an aqueous suspension concentrate composition comprising fumed alumina.
KR1020147013034A 2011-10-18 2012-10-17 Stable formulations containing fumed aluminum oxide KR101931846B1 (en)

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