Liquid pesticide composition

 

(57) Abstract:

The water composition pesticide-active substances with physical stability and high activity, contains the active substance - etofenprox, alachlor or trifluralin of 10.0 to 50.0 wt.%, surface-active polymer selected from the group of sodium salts of copolymers and takeaway acid and vinyl acetate or styrene and maleic acid, or polyacrylic acid is 0.01-10 wt.%, di-C10-C18-phthalate - 1.0 to 15.0 wt.% and water to 100 %. table 4.

The present invention relates to a liquid pesticide compositions with improved stability of the suspension, which is useful in the field of agriculture. More specifically, the present invention relates to compositions prepared in the form of a water suspension in which the water-insoluble physiologically-active substance with a melting point of from 15 to 70oC is in a stable dispersed state, so that no precipitation of crystals during storage.

Water-insoluble physiologically active substances as chemicals were used in the form of an emulsifiable concentrate or wettable powder, but recently they are often used as tekuceg the TCI chemicals, for example, water-insoluble pesticide, using a suitable dispersant. As a dispersing agent using a variety of anionic and nonionic surfactants, surfactant-based water-soluble polymers, and concentrate in suspension, has a stable form even under adverse storage conditions.

However, when using water-insoluble active substance with a melting point of from 15 to 70oC, during storage of the suspension concentrate in a sharp change of temperature, growth of crystals in the emulsified particles, and, thus, are such undesirable phenomena as the destruction of the emulsifying particles and precipitation of crystals.

Patent DE-A 3302648 describes the water dispersion of the suspension of agricultural concentrate, having a melting point 70oC and above, and other agricultural chemical having a melting point 70oC and below, optionally containing emulsifier and solubilizer1-12-alkylphenate. Furthermore describes that alkylphenate preferably has 4 to 8 carbon atoms, and most preferred example is dioctylphthalate. Opisyvaemaya-polyglycerol simple ester, containing 18 SW-links, (2) ethoxylated amine salts of poliakrilamidov, (3) simple polyglycolide esters of phenolaldehyde and (4) condensation products of alkylphenol with formaldehyde and polyamine a mixture of ionic and nonionic surfactants.

Patent DE-A 3304457 describes aqueous colloidal dispersion comprising an agricultural chemical and colloidal particles obtained by the polymerization of a hydrophobic monomer in the presence of the hydrophilic polymer. Both solutions differ from the proposals of the applicant in respect of dispersant chemical.

The compositions described in these sources, worse than proposed by the applicant from the point of view of stability, which is further confirmed by comparative examples 4-6 and 7-9, respectively.

As a means to stabilize emulsions were investigated: (1) the method where a hydrophilic protective colloid is reinforced by creating an ionic complex, (2) the method where the hydrophilic colloid obtained when the hydrophilic-hydrophobic interaction, and (3) the method where the change of the surface is achieved through the substance, which slightly differs in the magnitude of the solubility of the active substance. As a result, found that if the method (3) to use an ester of CFT is the Zia, in which will not involve the destruction of the emulsion or precipitation of crystals even during storage under such harsh conditions like the conditions established under cyclic test while keeping it in the range from high (50oC) to low (-10oC) temperature.

The present invention provides a liquid pesticidal composition, which comprises water-insoluble active substance in the form of fine particles with a melting point of from 15 to 70oC, water-soluble or vododispersionnoy polymer selected from the group: sodium salt of a copolymer basis of itaconic acid and vinyl acetate (1:0.1 to 20), the sodium salt of a copolymer of styrene and maleic acid (1:0.1 to 10), saponified copolymer of acrylic acid and vinyl acetate (1:0.5 to 10), polyacrylate sodium. The proposed composition contains an effective amount of pesticide, polymer in an effective amount as a dispersant, an ester of phthalic acid in an effective amount as an agent for preventing deposition of sludge and water in the following ratios, wt.

active substance 10,0 50,0

the polymer 0,01 10,0

di-C10-C18alkylphenate 1,0 15,0

water the rest

As an active substance in predpochtitelney a 2-(4-ethoxyphenyl)-2-methylpropyl 3-phenoxybenzyl ether.

Alachlor so pl. 41oC represents 2-chloro-2,6-diethyl-N-methoxyethylamine and trifluralin so pl. 49oC, ,,,-Cryptor-2,6-dinitro-N,N-DIPROPYLENE-toluidine, respectively.

In this invention to modify the surface layer in the proposed composition, the ester of phthalic acid is secreted onto the surface of the active substance, resulting receive a suspension having excellent stability during storage.

The invention is hereinafter described in detail with reference to the following examples, which in no way limit the scope of the proposed composition.

Below are the esters of phthalic acid and active ingredients, which are used in the examples given below.

(A) Esters of phthalic acid:

The compound (I)

< / BR>
Connection (2)

< / BR>
Connection (3)

< / BR>
Connection (4)

< / BR>
(C) Active substance: active ingredient (I) etofenprox, so pl. 37oC; active substance (II) alachlor, so pl. 41oC;

active substance (III) trifluralin, so pl. 49oC.

Example 1

A mixture consisting of 5 wt. parts of the compound (1) and 30 wt. parts of the active substance (1), melted, and then the melt is gradually poured into the solution, sod wt. parts of water, followed by stirring in a homogenizer, obtaining a suspension concentrate.

Comparative example 1

The melt of 30 wt. parts of the active substance (1) gradually pour in a solution containing 2 wt. part of the sodium salt of a copolymer basis of itaconic acid and vinyl acetate in 68 wt. parts of water, and after mixing in the homogenizer receive a suspension concentrate.

Example 2

A mixture consisting of 2 wt. parts of the compound (2) and 20 wt. parts of the active substance (1), is melted and the resulting melt is gradually poured into the solution containing 2 wt. part of the sodium salt of a copolymer of styrene and maleic acid (molar ratio 1/1) 76 wt. parts of water, and after mixing in the homogenizer receive a suspension concentrate.

Example 3

A mixture consisting of 10 wt. parts of compound (3) and 30 mass. parts of the active substance (II) is melted and the resulting melt is gradually poured into a solution containing 1.0 wt. part of the saponified copolymer of acrylic acid and vinyl acetate (molar ratio 1/1/), 0.5. parts polyoxyethyleneglycol sodium (5 mol) 58.5 wt. parts of water, and after mixing in the homogenizer receive a suspension concentrate.

Aut, and the resulting melt is gradually poured into a suspension prepared from 1 part by mass of sodium polyacrylate 54 wt. parts of water, and with stirring in a homogenizer receive a suspension concentrate.

Comparative example 2

The melt of 30 wt. parts of the active substance (III) gradually poured into a suspension containing 1 wt. part of the saponified polyvinyl acetate with a degree of saponification of 60% to 69 wt. parts of water, and after mixing in the homogenizer receive a suspension concentrate.

Comparative example 3

A mixture consisting of 15 wt. parts of the compound (IV) and 30 wt. parts of the active substance (III), melted and the resulting molten mixture was poured slowly into a solution containing 1 wt. part of dodecylbenzenesulfonate sodium and 2 wt. parts of polyethylene (12 mol) phenyl ester-modified styrene 52 wt. parts of water, and after mixing in the homogenizer receive a suspension concentrate.

Test for stability during storage

The concentrated suspensions obtained in accordance with examples 1 to 4 and comparative examples 1 to 3 are subjected to every test on the stability in storage, where one mode is maintained at a temperature of -10oC for rout in accordance with the following methods change the size of the particles, the change in viscosity, the presence or absence of a crystalline precipitate, change in content of the active substance and the change in the stability of the suspension.

Table 1 shows the data obtained.

Particle size is determined by the counter (coulter counter)

The viscosity is measured by Brookfield viscometer (30 rpm at 25oC).

The presence or absence of a crystalline precipitate checked with an optical microscope (magnification of 400 times).

The content of the active ingredient determined by gas chromatography.

The sample is placed in a cylinder with an inner diameter of 2 cm and a height of 10 cm, and according to the following formula to determine the ratio suspension:

< / BR>
where a represents the initial height of the suspension, and the mean height of the suspension after 20 cycles test.

Example 5

10 wt. parts of the compound (1) and 50 wt. parts of the active substance (1) mixed together and melted. The mixture is added to aqueous solution of 10 wt. parts copolymer basis of itaconic acid and vinyl acetate (ratio 1:5), having a degree of saponification of 50% in 30 wt. parts of water. The mixture is stirred for gommission getting dispersant chemical.

Example 6

1 wt. the connection part (1) and 10 by weight of the polymer basis of itaconic acid and vinyl acetate (ratio of 1:0,1), having a degree of saponification of 50% 88,9 wt. including water. The mixture is stirred using homosocial getting dispersant chemical.

Example 7

5 wt. including the compounds (1) and 10 wt.h. the active substance (I) is mixed with each other and melted. The mixture is added to aqueous solution of 0.01 wt.h. copolymer basis of itaconic acid and vinyl acetate (ratio 1:20), having a degree of saponification of 50% 84,99 wt.h. water. The mixture is stirred using a homogenizing mixer to obtain a dispersant chemical.

Example 8

5 wt. including di-isodecylphtalate and 10 wt.h. the active substance (II) are mixed together and melted. The mixture is added to aqueous solution of 0.01 wt.h. copolymer of acrylic acid and vinyl acetate (ratio 1:0.5), and having a degree of saponification of 50% 84,00 wt.h. water. The mixture is stirred using a homogenizing mixer to obtain a dispersant chemical.

Example 9

10 wt. including di-isodecylphtalate and 50 wt.h. the active substance (II) are mixed with each other and melted. The mixture is added to aqueous solution of 0.1 wt. including a copolymer of acrylic acid and vinyl acetate (ratio 1:10), having a degree of saponification of 50% of 39.9 wt.h. water. The mixture is stirred using a mixer to obtain a dispersant chemical.

Example 10

5 wt. o'clock with the ru 0,01 wt.h. polyacrylate sodium 84,99 wt.h. water. The mixture is stirred using a mixer to obtain a dispersant chemical.

Example 11

10 wt.h. compounds (3) and 50 wt.h. the active substance (III) mixed together and melted. The mixture is added to aqueous solution of 0.1 wt.h. polyacrylate sodium 39.9 wt.h. water. The mixture is stirred using a mixer to obtain a dispersant chemical.

Comparative example 4

20 wt. hours of dioctylphthalate and 30 wt.h. the active substance (I) is mixed with each other and melted. The mixture is added to aqueous solution of 5 wt.h. product Soprophor FL and 5 wt.h. polyvinyl acetate 40 wt.h. water. The mixture is stirred using a homogenizing mixer to obtain dispersant. "Soprophor FL" is a trade name for triethanolamine salt mixture is complex postinoculation of monoether and diapir christiantheologians ether containing 18 ethylenoxide links and is described in DE-A 3302648, page 7, lines 1 to 4.

Comparative example 5

15 wt. hours of dioctylphthalate and 15 wt.h. the active substance (II) are mixed together and melted. The mixture is added to aqueous solution of 5 wt.h. product Soprophor FL and 5 wt.h. polyvinyl acetate 60 wt.h. water. The mixture is stirred using homogenizer and 10 wt.h. the active substance (III) mixed together and melted. The mixture is added to aqueous solution of 5 wt.h. product Soprophor FL and 5 wt.h. polyvinyl acetate 75 wt.h. water. The mixture is stirred using a homogenization mixer to obtain a dispersant chemical.

Comparative example 7

1 kg (5 wt.h.) 20% aqueous solution of polyethylene glycol are placed in a round bottom glass flask and heated to 80oC. Under stirring drops for the start of the polymerization, add 250 g of ethyl acrylate and 20 g of a 5% aqueous solution of ammonium persulfate. The addition continued for 2 hours. The reaction mixture is allowed the opportunity to stand at 80oC for one hour to place the remaining monomer. The mixture of products is cooled to room temperature and treated on the filter, 100 mesh (the Japanese. the NAC. standard) to correct coagulation and obtain aqueous colloidal dispersion. 700 g of the dispersion is mixed with water to produce 1 kg of the diluted product. During mixing to dispersion for 3 minutes add 800 g of molten physiologically active substances (1). Stirring is continued for another 30 minutes to obtain a dispersant chemical.

Comparative example 8

700 g of a dispersion, polucheniya to dispersion for 3 minutes, add 500 grams of molten physiologically active substance (II). Stirring is continued for another 30 minutes to obtain a dispersant chemical.

Comparative example 9

700 g of the dispersion obtained in comparative example 7, is mixed with water to produce 1 kg of the diluted product. During mixing to dispersion for 3 minutes, add 300 g of molten physiologically active substance (III). Stirring is continued for another 30 minutes to obtain a dispersant chemical.

Test 5 stabilization

The dispersant obtained in examples 5 to 11 and comparative examples 4 to 9, are studying in the same manner as in test 1 for stability. The results are shown in table. 1.

Example 12

Mix with each other 5 wt. including the compounds (1) and 10 wt. including the active substance (1) and melted. The mixture is added to aqueous solution of 1 wt. including a copolymer of acrylic acid and vinyl acetate (molar ratio 1:20), having a degree of saponification of 50% to 80 wt. including water. The mixture is stirred at gammexane to obtain a dispersing agent.

Example 13.

Mix with each other 5 mass parts of the compound (1) and 30 wt. including the active substance (1) and melted. The mixture is added to aqueous solution of 2 wt. including a copolymer of styrene and maleic acid (tx2">

Example 14

Mix with each other 5 wt. including the compounds (1) and 30 wt. including active compounds (1) and melted. The mixture is added to aqueous solution of 2 wt. including a copolymer of styrene and maleic acid (molar ratio 1:5) 60 wt. including water. The mixture is stirred at gammexane to obtain a dispersing agent.

Example 15

Mix with each other 5 wt. including compounds 1 and 30 wt. including the active substance (1) and melted. The mixture is added to aqueous solution of 2 wt. including a copolymer of styrene and maleic acid (molar ratio 1:10) 60 wt. including water. The mixture is stirred at gammexane to obtain a dispersing agent.

Test 2 on herbicide action

Prepared according to the method of example 4 a suspension of trifluraline and control emulsion below, each diluted in 300 and 500-fold. To 7 ml per pot size 12 cm in diameter, were taken from each of the diluted dispersion is sprayed on plants, growing up to 7 cm Rosicky blood in the blooming phase of the second or third leaf planted on 30 pieces to the pot. After 14 days, the fresh weight of the remaining above-ground parts of Rosicky measure and determine the degree of herbicide activity when compared to untreated the spending containing 30 wt. parts trifluraline, 60 wt. parts of xylene and 10 wt. parts of emulsifier, consisting of 32 wt. dodecylbenzenesulfonate calcium, 48 wt. polyoxyethylene (10) simple nonylphenylether ether and 20 wt. polyoxyethylene (10) complex sorbifolia ether.

Test 3 insecticidal activity

In a pot the size of 1/10,000 grown plant rice before buds 4 piece, and then on a rotating table to sprinkle on him dispersion prepared in example 1 and diluted to the following concentrations in a dose of 50 ml per 3 pots. Through 1,3,5 or 8 days, this plant cover cylindrical wire mesh and inside each covered with a mesh pot plant with the free mixing of 10 adult females of cicadas green rice and 10 adult females small delfinado. After 24 hours, the dead insect count and receive the degree of insecticidal action on average about 3 pot. Table 3 summarizes the data obtained.

Control emulsifiable concentrate experience, according to the above method. The specified control concentrate consists of 21.5 wt. parts of the active substance (1), 6 wt. parts Solpol T LL (trade name), manufactured filterresults calcium and 83.5 wt. parts of xylene.

The data obtained show that the proposed composition (preparation) for agriculture is superior to the insecticidal action of the control concentrate.

Test 4 on insecticidal activity.

The test sample And receive according to the method described in example 1 and processed as described in test 1. Separately receive the sample by the same method as described in example 1, but without processing it. Both sample a and b have a similar way, as shown in test 3. The results are shown in table 4.

The data obtained show that the proposed composition continues to be biocidal action, even after a certain period of storage. TTT

Liquid pesticide composition comprising an active ingredient, a polymeric dispersant, and water, characterized in that the active substance it contains etofenprox, or alachlor, or trifluralin, as a polymeric dispersant polymer selected from the group of sodium salt of a copolymer basis of itaconic acid and vinyl acetate 1 0,1 20, the sodium salt of a copolymer of styrene and maleic acid 1 0,1 10, saponified copolymer of acrylic acid and vinyl acetate 1 0,5 10, Poliakov, wt.

Active substance 10,0 50,0

Polymer dispersant 0,01 10,0

Di-C10-C18-alkylphenate 1,0 15,0

Water The Rest

 

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