Pesticide composition

FIELD: organic chemistry, pesticides.

SUBSTANCE: invention relates to concentrated pesticide solution, containing 0.5-50 mass/vol.% one or more water insoluble pesticides and lignin in mass ratio lignin/pesticide of 1:10-1:1, dissolved in polar solvent mixable with water in amount to adjust total volume to 100 %. Dispersed in water concentrated pesticide solution is applied onto pests or locus thereof.

EFFECT: storage stable products.

9 cl, 7 tbl, 2 ex

 

This invention relates to compositions of pesticides and, more specifically, to concentrated solutions of water-insoluble pesticides. It also relates to the production of data concentrated solutions and their use in diluted form.

Pesticides that have low solubility in water and which is chemically stable in water, are usually available in industrial aqueous suspensions of concentrates (SC) and diluted for use in a production environment. Suspended as a pesticide active ingredient must have a small particle size in order to maintain the suspended state when stored in the form of a concentrate and upon further dilution with water. For this purpose, as a rule, it is necessary to crush the active ingredient, but this process takes time and is costly. Even so, there are often problems associated with suspensions concentrates, resulting in the deposition of particles during long-term storage, counter-precipitated particles to resuspending and sometimes increase the size of the particles of the active ingredient during storage.

One alternative is the dissolution of water-insoluble active ingredient in a water-immiscible solvent such as an aromatic hydrocarbon, getting emulge is budegassa concentrate (EC). It can be stored in the form of a stable solution, and dilute with water before applying the emulsion milky color with a small particle size. Water-insoluble pesticides, which are poorly soluble in normal water-insoluble solvents, can be dissolved in a miscible with water, the solvent to form stable when stored soluble concentrate (SL). Pesticide forms a suspension upon dilution with water. For example, in the publication WO 92/10937 described soluble concentrates of this type. Data SL are three-component composition in which a solid water-insoluble pesticide and dispersant are solubilizing form in mixing with the water solvent. You can mention a dispersant comprising a polymer alkylated vinylpyrrolidone, condensates ethylene oxide-propylene oxide/propylene glycol, adducts of Nonylphenol-ethylene oxide and various ethoxylates. Solvents include acetonitrile, α-butyrolactone, dimethylketone, dimethylfuran, dimethylsulfoxide, methanol and N-organic.

The lack of application of water-soluble solvents for dissolving the active ingredients of low solubility in water are their weak properties of dilution water. Often the active ingredient is quickly deposited in the form of large crystals that bring the to a number of problems when using, such as clogging of the spray filter or nozzle and low or unstable biological effectiveness. To prevent, or more frequently slow deposition inclusion of excess emulsifying or dispersing agent, usually in a 1:1 ratio with the active ingredient, but at these concentrations of surfactants having problems with phytotoxicity due to them.

In accordance with the present invention provides a concentrated solution of the pesticide, which includes one or more water-insoluble pesticides and lignin dissolved in the mixing water of the polar solvent.

The pesticide or pesticides used in the concentrated solution according to the invention are water-insoluble compounds and can be solid or liquid, but the invention is of particular value for pesticides, which are solid compounds at room temperature. Usually they have a solubility in water of no more than 0.2% wt./about. They should also be dissolved in the selected miscible with water is a polar solvent.

The used quantity of the pesticide or pesticides, as a rule, will be from 0.5 to 50% wt./about., preferably from 1 to 30% wt./about. and usually from 5 to 20% wt./about., to the solution as a whole.

Pesticides include gerbic the water, insecticides and fungicides. The invention is particularly suitable for any pesticide or mixture of pesticides, having a solubility in water of no more than 0.2% wt./about. Examples of pesticides for use in this invention are napropamide, haloxyfop, gladiatorial, mesotrione, cypermethrin, alpha-cypermethrin, beta-cypermethrin, tsyprokonazolu, difenoconazol, hexaconazole, penconazole, tebuconazole, AZOXYSTROBIN, picoxystrobin, kresoxim-methyl, metamyosyn, pyraclostrobin, Trifloxystrobin, cyprodinil, metalaxyl, mefenoxam, fluazinam, fludyoksonil paclobutrazol, thiabendazol and quinoxyfen. However, the invention is particularly suitable for fungicides, especially fungicides on the basis of a triazole fungicide, and on the basis of strobilurin, and for mixtures of fungicides, especially for mixtures of fungicides on the basis of strobilurin, for example, picoxystrobin with fungicide on the basis of a triazole such as hexaconazole or tsyprokonazolu. Of particular interest are concentrated solutions prepared from fungicide, selected from the group consisting of AZOXYSTROBIN, picoxystrobin, tebuconazole, cyproconazole and picoxystrobin mixed with cyproconazole.

Under the lignin refers to the lignin in the form of the free acid, but not in the form of alkali metal salt of lignin such as sodium salt, or lignosulfonate. Lignin, which p is ecstasy a polymer phenylpropene different molecular weight, can be obtained from the spent liquor of the sulfate and soda processes used in the woodworking industry. Thus obtained lignin known as alkali lignin, additionally referred sulfate (or Kraft) lignin or soda lignin. Of particular applicability for use in the present invention has indulin at (indulin the ATA is a trade name), which is a highly purified lignin obtained from black liquor pine trees and prepared in the form of loose brown powder.

The amount of lignin used in a concentrated solution of the present invention, in relation to the number of the pesticide used in the mass ratio is from 1:10 to 1:1, usually from 1:8 to 1:2, preferably from 1:6 to 1:4 and 1:5 of lignin to the total weight of the pesticide.

In the invention can use any miscible with water, a polar solvent which can dissolve as a pesticide, and lignin. Suitable solvents include γ-butyrolactone, tetrahydrofurfuryl alcohol, N-organic, dimethylsulfoxide, N,N-dimethylformamide and ethyllactate. Preferred solvents are γ-butyrolactone and tetrahydrofurfuryl alcohol, and N-organic is a particularly preferred solvent. WMS is about to use a mixture of polar solvents, for example, a mixture of N-organic-poly(ethylene glycol)200 in the ratio of 50:50. The amount of solvent used should be sufficient to obtain the General solution to 100% wt./about.

Although it is insignificant, but concentrated solution may include additives, such as polymer stabilizers or means of preventing the deposition, to improve the dissolution. Examples of polymeric stabilizers or means preventing the deposition, include water-soluble and water-insoluble polymers such as ethylcellulose, casein, hydroxypropylcellulose, AvicelTMCL-611 (based on microcrystalline cellulose), AgrimerTMVEMA AN-216 (copolymer of vinyl ether maleic anhydride with a molecular mass of 55000-80000), NU-FILM-PTM(poly-1-p-menthene) and KelsenTM(xanthan gum). Such additives are usually used in amounts up to 0.5% wt./about., for example in the range from 0.1 to 0.4% wt./about., as a rule of 0.25% wt./about. to the total weight of the composition, depending on their solubility in the used polar solvent. For example, the maximum number of Avicula CL-611 and Kelzan, which can be dissolved in the concentrate based on N-methylpyrrolidone is about 0.1% wt./about.

In one variant embodiment of the invention provides a concentrated solution of a pesticide that contains:

(and from 1 to 30% wt./about., usually from 5 to 30% wt./about. and usually from 10 to 20% wt./about. one or more water-insoluble pesticides and

(b) lignin mass ratio of from 1:10 to 1:1, usually from 1:8 to 1:2 and preferably from 1:6 to 1:4, usually 1:5, to the component (a), where both components (a) and (b) dissolved in a miscible with water, polar solvent (s) such as γ-butyrolactone, tetrahydrofurfuryl alcohol, ethyllactate and, preferably, N is the organic.

In this variant embodiment of a concentrated solution optionally contains up to 0.5% wt./about. other additives such as a stabilizer or a means of preventing the deposition of, for example, ethylcellulose.

A concentrated solution according to the invention is prepared by dissolving the pesticide or pesticides, lignin and, optionally, stabilizers, and other additives, in a polar solvent. Ingredients can be added to the solvent in any order. This is usually performed at room temperature with a corresponding shaking or stirring. To ensure dissolution of the solvent can be heated to a temperature of, for example, 50°C.

When a concentrated solution is ready for use, it is diluted with water, usually by adding the solution to mix the volume of water to obtain a water dispersion of the pesticide or pesticides containing, for example, from 0.0001 to 1% wt./about. Pesti is IDA or pesticides. Then aqueous pesticide solution is applied by spraying or other known method in place to be processed.

Thus, an additional variant embodiment of the present invention provides a method of destroying or pest plants, which comprises applying to the pest or a place affected by the pest, effective as of pesticide quantity of water dispersion obtained by dispersing in water the concentrated pesticide solution according to the invention.

The advantage of concentrated solutions of the pesticides of the present invention is that they can provide sub-micron (about 0.4 μm) mainly monodisperse particles when dissolved in water, which is stable against subsequent increase in size, at least within 24 hours

The invention is illustrated by reference to the following examples. In the examples the following abbreviations are used:

ai = active ingredientSL = soluble concentrate
ppm = part per millionw/v = weight/about.
w/w = weight/wt.init = original

DMSO = dimethyl sulfoxide
NMP = N-organicGBL = γ-butyrolactone
THFA = tetrahydrofurfuryl alcohol
PEG 200 = poly(ethylene glycol), average molecular weight 200
EL = ethyllactate.

Example 1

This example shows how to determine the size of the particles, when concentrated solutions of pesticides obtained according to the present invention is diluted with water. The results are presented for a number of solutions according to the invention.

Test method variance

The compositions were tested against dispersing properties in water by adding 2.5 ml of solution concentrate in a pipette into a closed tube tank Crow, with a 97.5 ml of standard hard water CIPAC. Noted the original "blurred" when making the first few drops in the water, then the tank turned 3 times and noted the homogeneity of the dispersion. Determination was carried out at set intervals for 24 h to assess any deposition or crystallization.

Determination of particle sizes in dilutions initially and after 24 h was performed using the following parameters of the device Malvern Mastersizer S.:

Polydisperse modelDefined values of particle size:
Darkening 2-4%Volumetric CPE is ion battery diameter

D (v, 0,5)
The pump speed 40%Volume average diameter

D [4,3]

The mixing rate 20%% of particles with size less than 1 micron
Ultrasound - no

Used types of standard hard water was a CIPAC and CIPAC C. They have the following characteristics:

CIPAC: hardness 20 ppm; pH 5.0 to 6.0; Sa2+Mg2+= 1:1;

CIPAC WITH: the hardness of 500 ppm; pH 7,0-8,0; CA2+Mg2+= 4:1.

(a) Soluble concentrates of AZOXYSTROBIN

Preparing compositions SL containing 10% wt./about. AZOXYSTROBIN in NMP and various concentrations of lignin, and were evaluated on the properties of cultivation. In tables 1 and 2 below presents the results.

Table 1

Breeding AZOXYSTROBIN in CIPAC water AND
Indulin at, % wt./about.Originally in the water CIPAC AAfter 24 h in water CIPAC A
AverageMedian% of particles <1 μmAverageMedian% of particles <1 μm
19,710,4485,69 0,390,37100,00
2of 3.460,3890,561,250,3995,68
30,400,38100,000,390,37100,00
50,390,37100,000,380,36100,00
102,770,3876,314,510,4170,43

Table 2

Breeding AZOXYSTROBIN in CIPAC water
Indulin at, % wt./about.Originally in the water WITH CIPACAfter 24 h in water WITH CIPAC
AverageMedian% of particles <1 μmAverageMedian% of particles <1 μm
1---0,880,3894,11
21,390,3788,050,530,3996,58
30,740,3893,62 1,960,4183,11
51,330,4087,7685,440,6164,38
105,140,9051,937,151,9039,38

The results indicate that to maintain the particles in finely ground condition, the optimal concentration of indulin at approximately 2-3%.

At a concentration of 5-10% observed the formation of flakes after 24 h, especially in CIPAC water WITH what was reflected in higher values of the average particle size and the reduction in the percentage of particles with size less than 1 micron.

(b) Soluble concentrates picoxystrobin

Prepared 10% wt./wt. composition SL in NMP containing 1, 2 and 5% wt./about. lignin and dilutions were determined by particle size in 24 hours the Results are presented in table 3.

Table 3

Breeding picoxystrobin
Indulin at, % wt./about.In CIPAC water AIn CIPAC water
AverageMedian% of particles <1 μmAverageMedian% of particles <1 μm
1 14,010,5676,3223,810,6865.22 per
21,690,5184,291,110,5281,21
51,780,4686,541,160,5773,57

(C) Soluble concentrate of tebuconazole

Prepared 10% wt./about. composition SL in NMP containing 5% lignin. After 24 h was obtained by dilutions are presented in table 4.

Table 4

Breeding of tebuconazole
Indulin at, % wt./about.In CIPAC water AIn CIPAC water
AverageMedian% of particles <1 μmAverageMedian% of particles <1 μm
50,360,35100,000,370,36100,00

(d) Soluble concentrate cyproconazole

Prepared 10% wt./about. composition SL in NMP containing 5% lignin.

The results are presented in table 5.

Table 5

Breeding cyproconazole
Indulin at, % wt./about.In CIPAC water AIn CIPAC water
AverageMedian% of particles <1 μmAverageMedian% of particles <1 μm
514,410,3578,9014,220,3382,39

(e) Soluble concentrate mixture picoxystrobin/tsyprokonazolu

Prepared composition SL (12.5% wt./about. picoxystrobin and 5.0% wt./about. cyproconazole containing 8% wt./about. lignin. After 24 h were obtained by breeding, are presented in table 6.

Table 6

Dilution of the mixture picoxystrobin/tsyprokonazolu
Indulin at, % wt./about.In CIPAC water A
AverageMedian% of particles <1 mm
83,500,4680,33

Example 2

This example shows the use of alternative polar solvents to obtain concentrated solutions according to the invention and the use of other is their pesticides.

Preparing compositions SL containing 10% wt./wt. the active ingredient and 4% wt./wt. indulin at using the active ingredients of AZOXYSTROBIN, hexaconazole, cypermethrin and mesotrione with NMP as solvent. In addition, prepared for a similar composition of AZOXYSTROBIN with the following solvents: γ-butyrolactone, DMSO, tetrahydrofurfuryl alcohol, ethyllactate and a mixture of 50% N-organic/50%/PEG-200.

Cultivation of these songs (2500 ppm of active ingredient in water WITH CIPAC) was tested by the method described in example 1, with results shown in table 7.

Table 7

Alternative solvents
SolventQuality breeding time (hour)Retention on the sieve (75 µm)
Original0,51,02,03,06,024,0
N-methyl-pyrrolidone*******no
γ-butyrolactone*******no
DMSO*******no
Tetrahydrofurfuryl alcohol*******no
Ethyllactate*******no
N-organic/PEG*******no
*Suspension of fine sub-micron particles

These results indicate that all the combinations of active ingredients and solvents gave satisfactory cultivation within 24 hours of obtaining small suspension passing through a sieve with a pore size of 75 microns.

1. Concentrated pesticide solution containing one or more water-insoluble pesticides and lignin dissolved in a miscible with water, a polar solvent, in which the amount of pesticide or pesticide is from 0.5 to 50% wt./vol.; the amount of lignin in the mass ratio is from 1:10 to 1:1 lignin to the total quantities of the pesticide and the amount of solvent used is sufficient to bring the total solution to 100%.

2. Concentrated pesticide solution according to claim 1, in which the pesticide is a fungicide on the basis of strobilurin or fungicide on the basis of a triazole or a mixture.

3. Concentrated pesticide solution according to claim 2, in which the pesticide is a fungicide selected from the group consisting of AZOXYSTROBIN, picoxystrobin, tebuconazole, cyproconazole and picoxystrobin mixed with cyproconazole.

4. Concentrated pesticide solution according to any one of the preceding paragraphs, in which the polar solvent is selected from the group consisting of γ-butyrolactone, tetrahydrofurfuryl alcohol, ethyllactate and N-methylpyrrolidone.

5. Concentrated pesticide solution according to any one of the preceding paragraphs which includes a polymeric stabilizer or remedy for preventing the deposition.

6. Concentrated pesticide solution according to claim 5, in which the polymer stabilizer or remedy for preventing the deposition, is ethylcellulose.

7. Concentrated pesticide solution, which contains:

(a) from 1 to 30% wt./about. one or more water-insoluble pesticides and

(b) lignin mass ratio of from 1:10 to 1:1 to the total number of the pesticide, where both components (a) and (b) dissolved in a miscible with water, polar solvent, and the amount used is wow solvent is sufficient to bring the total solution to 100%.

8. Concentrated pesticide solution according to claim 7, which contains up to 0.5% wt./about. polymer stabilizer or means of preventing the deposition.

9. Way to destroy or control pests of plants, which comprises applying to the pest or lesion pest effective as a pesticide, the amount of water dispersion obtained by dispersing in water a concentrated solution of the pesticide according to any one of the preceding paragraphs.



 

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2 cl, 4 tbl, 2 ex

FIELD: organic chemistry, agriculture, herbicides.

SUBSTANCE: invention describes a herbicide agent containing the effective amount of a mixture of active substances and comprising: (a) substituted arylsulfonylaminocarbonyl-triazolinone of the formula (I): wherein R1 means alkyl comprising up to 6 carbon atoms; R2 means alkoxy-group comprising up to 6 carbon atoms; R3 means alkoxycarbonyl or alkoxy-group substituted with halogen atom and each comprising up to 6 carbon atoms; R4 means hydrogen atom, and also salts formed by compound of the general formula (I) with basic compounds (compound of the group 1), and (b) compound improving the tolerance of crop plants to herbicides effect and chosen from the following group of compound of the general formula (II): wherein m = 1; n = 0; X means alkoxy-group comprising up to 6 carbon atoms; Z means a group , wherein R5 means hydrogen atom; R6 means alkyl comprising from 1 to 6 carbon atom and substituted with (C1-C4)-alkoxy-group (compounds of the group 2) in the weight ratio of compound of the group 1 to compound of the group 2 = (1:12.5)-(1:50), and a method for control of weed plants using the proposed herbicide agent. Invention provides good tolerance of crop plants in their treatment with the proposed herbicide agent.

EFFECT: improved and valuable properties of agent.

8 cl, 5 tbl, 1 ex

Rodenticide agent // 2289925

FIELD: rodenticides.

SUBSTANCE: invention relates to agents used for control of mouse-like rodents. Rodenticide agent comprises an active substance, attractant, dye, repellent agent for humans and domestic animals and a binding component. Thermoplastic is used as a binding component and agent comprises components taken in the following ratio, wt.-%: active substance, 0.002-10; attractant, 40-85; dye, 0.005-0.05, repellent for humans and domestic animals, 0.001-0.02, and a binding agent, the balance. Invention provides enhancing the mechanical strength of agent at increased temperatures and its moisture resistance. Invention can be used for carrying out the deratization of compartments and in agriculture also.

EFFECT: enhanced effectiveness of agent.

3 tbl

FIELD: organic chemistry, chemical technology, medicine, pharmacy.

SUBSTANCE: invention relates to a novel terbinafine salt of the formula (I):

with malic acid possessing an antimycotic activity and to a method for its preparing and pharmaceutical composition used in treatment of fungal infection. L-(-)-bimalate is the most preferable form of salt. Method for preparing salt involves interaction of compound of the formula (I) as a free base with the corresponding form of malic acid. Pharmaceutical composition comprises indicated salt in combination with at least one pharmaceutically acceptable carrier or excipient. Pharmaceutical composition can be prepared as a solution or lacquer for nails. Proposed salt shows improved pharmacokinetic properties that makes its to be preferable in preparing pharmaceutical compositions adopted for systemic and topical using.

EFFECT: improved preparing method, improved and valuable properties of salt and pharmaceutical composition.

8 cl, 6 dwg, 5 ex

FIELD: pesticides, chemical technology.

SUBSTANCE: invention describes a method for preparing copper-containing liquid pesticide. Method involves formation of a hardened water-soluble complex copper-borate, its grinding to form granules and dissolving granules in water to obtain liquid pesticide comprising the copper concentration at least 0.20% but not above 1.00 wt.-%. Also, invention describes liquid pesticide prepared by indicated method and a set comprising granules of hardened water-soluble complex copper-borate and letter instructions for preparing the liquid pesticide. Method provides remaining copper in solution in dissolving the hardened complex copper-borate in water.

EFFECT: improved preparing method.

4 cl, 1 dwg

FIELD: organic chemistry, chemical technology.

SUBSTANCE: invention describes {[1-(ammonio)-3,5,7-triazaadamantyl]methylcarbonyloxypoly-(alkyleneoxy)}-propane chlorides of the general formula: wherein at X+ = Y+ means ; R1 means aliphatic unsaturated hydrocarbon C17-radical; a + c + e = 49; b + d + f = 9; at X+ = Y+ means ; R1 means aliphatic unsaturated hydrocarbon C17-radical; a + c + e = 55; b + d + f = 10; at X+ = Y+ means ; a + c + e = 49; b + d + f = 9; at X+ = Y+ means ; a + c + e = 55; b + d + f = 10; at X+ = Y+ means ; R1 means aliphatic unsaturated hydrocarbon C17-radical; a + c + e = 49; b + d + f = 0; at X+ = Y+ means ; R1 means aliphatic unsaturated hydrocarbon C17-radical; a + c + e = 55; b + d + f = 0; at X+ = Y+ means -RNH2+-; R means aliphatic hydrocarbon (C10-C16)-radical; a + c + e = 49; b + d + f = 9; at X+ = Y+ means -RNH2+-; R means aliphatic hydrocarbon (C10-C16)-radical; a + c + e = 55; b + d + f = 10. Also, invention describes a method for synthesis of abovementioned compounds that possess antibactericidal and fungicide activity and can be used for control of bacterial and fungal damages in medicine, veterinary science and agriculture.

EFFECT: improved method of synthesis, valuable properties of compounds.

7 cl, 2 tbl, 8 ex

FIELD: agriculture, organic chemistry.

SUBSTANCE: invention relates to agent for pest and acaridae controlling containing mixture of a) compound of formula I , wherein X represents C1-C4-alkyl; W, Y, and Z are independently hydrogen or C1-C4-alkyl; A and B together with the hydrogen atom to which they are attached form saturated C3-C6-cycloalkyl monosubstituted with (C1-C4-alkoxyl; D represents hydrogen; G represents hydrogen or group , wherein M is oxygen; R2 is C1-C8-alkyl; and b) compound selected from group containing acrinatrin, cypermetrin, alpha-cypermetrin, zeta-cypermetrin, cyflutrin, beta-cyflutrin,, deltametrin, lambda-cyhalotrin, phempropatrin, and biphentrin, wherein a) and b) mass ratio is from 25:1 to 1:1.

EFFECT: agent with synergic effect and increased activity.

3 cl, 12 tbl, 5 ex

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