DE3702604A1 - Liquid pesticide and process for its preparation - Google Patents

Abstract

The invention relates to a liquid pesticide in the form of an aqueous dispersion which contains one or more active substances with a melting point of below 70@C and one or more active substances with a melting point of above 70@C. In contrast to previously known mixed dispersions, the novel preparation does not contain any organic solvent. It is environmentally friendly and economical.

Description

The invention relates to liquid pesticide agents in the form of aqueous dispersions that are at least one below of 70 ° C melting active ingredient and at least one above contain from 70 ° C melting active ingredient.

The following substances are active substances with a Melting point above 70 ° C particularly suitable.

Herbicide urea derivatives, such as
Isoproturon [N, N-dimethyl-N ′ - (4-isopropyl-phenyl-) urea],
Linuron [N- (3,4-dichlorophenyl) -N'-methoxy-N'-methylurea],
Monolinuron [N- (4-chlorophenyl) -N'-methoxy-N'-methylurea] and
Diuron [N- (3,4-dichlorophenyl) -N ′, N′-dimethylurea]

herbicide triazine derivatives, such as
Atrazine [2-chloro-4-ethylamino-6-isopropylamino-1,3,5-triazine],
Cyanazine [2- (4-chloro-6-ethylamino-1,3,5-triazin-2-ylamino) -2-methylpropionitrile] and
Simazine [2-chloro-4,6-bis-ethylamino-1,3,5-triazine],

fungicidal active ingredients, such as
Fentin hydroxide (triphenyltin hydroxide),
Carbendazim (methylbenzimidazol-2-ylcarbamate),
Captafol [3a, 4,7,7a-tetrahydro-N- (1,1,2,2-tetrachloroethylthio) phthalimide and

as an insecticidal active ingredient
Endosulfone- (6,7,8,9,10,10-hexachloro-1,5,5a, 9a-tetrahydro-6,9-methano-2,4,3-benzo-dioxa-thiepinoxide).

The following substances are active substances with a Melting point below 70 ° C particularly suitable.

Herbicide active ingredients, such as
Trifluralin [2,6-dinitro-N, N-dipropyl-4-trifluoromethyl-aniline],
Pendimethalin [N- (1-ethylpropyl) -2,6-dinitro-3,4-xylidine],
Dinoseb acetate (O-acetyl-2-sec-butyl-4,6-dinitrophenol),
Dowco 433 [4-amino-3,5-dichloro-6-fluoro-2-pyridinoxyacetic acid isooctyl ester] and

herbicide phenoxypropionic acid esters, in particular
Diclofop-methyl [2- (4- (2,4-dichlorophenoxy) phenoxy) propionic acid methyl ester],
Ethyl 2- (4- (6-chloro-2-benzoxazoyloxy) phenoxy) propionate,
Ethyl 2- (4- (6-chloro-2-benzothiazolyloxy) phenoxy) propionate and

as a fungicidal active ingredient
Pyrazophos [2-O, O-diethylthionophosphoryl) -5-methyl-6-carbethoxy-pyrazolo [1,5-a -] - pyrimidine].

The previously listed active ingredients and active ingredient mixtures are from EP 01 17 999 B1 as liquid pesticide agents known on the basis of aqueous mixed dispersions. The Known agents contain an active ingredient concentrate or several active ingredients melting below 70 ° C of phthalic acid (C₁-C₁₂) alkyl esters as solvents in Combination with an aqueous suspension concentrate or several active ingredients melting above 70 ° C.

Furthermore, the active substances mentioned are partly in H. Martin.  The Pesticide Manual, British Crop Protection Counsel, 6th edition, 1979. The two benzoxazolyl and Benzothiazolyl-phenoxy propionic acids are from DE-OS 26 40 730 known, and Dowco 433 (4-amino-3,5-dichloro-6-fluoro-2-pyridine-oxylacetic acid isoctyl ester is in the European patent application 67 712.

The tank mixes commonly used up to now have the disadvantage that the combined formulations of Active ingredients were often incompatible. That resulted in practice to segregation or to agglomerate formation, which the spray nozzles clog.

These disadvantages were overcome by the preparations according to the EP 01 17 999 overcome. The active ingredient combinations mentioned there have also proven themselves in practice as valuable pesticides.

However, these liquid pesticidal agents have the disadvantage that they contain phthalic acid (C _1-12 ) alkyl esters as solvents. The esters are placed with the end product, for example on the soil or the plants. This not only wastes the expensive solvents, it also creates an additional burden on the environment.

The object of the invention is to overcome the disadvantages mentioned above to overcome and new pesticide means in the form of watery  To provide dispersions that have one or more active ingredients melting below 70 ° C and one or more Active ingredients melting above 70 ° C, but not organic Contain solvents. The new pesticide preparations should therefore be cheaper and more environmentally friendly.

According to the invention, this task is accomplished by a pesticidal agent dissolved, in which the active ingredient (s) melting below 70 ° C as a dispersion in water in combination with an aqueous suspension concentrate above 70 ° C melting active ingredients are present.

To the group of active ingredients used according to the invention a melting point below 70 ° C include trifluralin, pendimethalin, dinoseb acetate, diclofopmethyl, pyrazophos and (4-Amino-3,5-dichloro-6-fluoro-2-pyridine) isooctyl oxylacetate.

To the group of active ingredients used according to the invention a melting point above 70 ° C include endosulfone, diuron, Atrazin, Cyanazin, Simazin, Isoproturon, Linuron, Captafol, Carbendazim and fentin hydroxide.

Preferred examples of active substance combinations are alizarin / Pendimethanol, Diuron + Atrazin / Pendimethalin, Diuron + Atrazin / Pendimethalin + trifluralin, isoproturon / trifluralin, linuron / Diclofopmethyl, carbendazim / pyrazophos, endosulfan / pyrazophos, Cyanazin / Pendimethalin and Simazin / Trifluralin.

The active ingredient combination of atrazine is particularly preferred (2-chloro-4-ethylamino-6-isopropylamino-1,3,5-triazine) and  Pendimethalin (N- (1-ethylpropyl) -2,6-dinitro-3,4-xylidine).

The pesticide agent according to the invention preferably contains a dispersant and / or a wetting agent and optionally other additives and / or auxiliaries.

Surprisingly, it was found that in the manufacture an effective liquid pesticide an organic Solvent by water as the liquid phase of a dispersion can be replaced. This not only saves costs, but also the environmental impact is reduced. For this purpose, the active ingredient melting at more than 70 ° C in Water dispersed together with additives and / or auxiliaries, and the active ingredient melting at less than 70 ° C is melted in a water bath and into the Sprayed dispersion.

Spraying the melted active ingredient into the cooled Suspension of the first active ingredient has the advantage that the Crystallize sprayed droplets quickly. By the subsequent Wet grinding becomes a particle size distribution of about 95% <8 µ. This is for storage stability dispersion is essential. With the mentioned particle size becomes a storage stability of the homogeneous dispersion over many Months if the storage temperature is not around 30 ° C exceed. The formulations are biologically active and have no phytotoxicity.  

Rhodopoly and water also contribute to the fact that no active ingredient particles settle out of the dispersion.

The pesticide agent according to the invention preferably contains 5 to 50% by weight of the active ingredient melting below 70 ° C. and 5 to 50% by weight of the active ingredient melting above 70 ° C. and 2 up to 20% by weight of emulsifier and in each case less than 1% by weight of antifoam, Formalin and polysaccharide.

Triethanolamine salts of a mixture are preferably used as emulsifiers of phosphoric acid mono- and diesters of a tristyryl polyglycol ether with 18 EO units, amine salts of ethoxylated polyacrylphenols, polyglycol ethers of a phenol aldehyde, Condensation products of alkylphenols with formaldehyde and polyamines or a mixture of ionic and non-ionic surfactants.

A preferred embodiment of the pesticide according to the invention Means has the following components:

20-30% by weight pendimethalin 15-25% by weight atrazine 2-5% by weight monoethylene glycol 5-10% by weight emulsifier 0.2-1.0% by weight of anti-foaming agent 0.1-1.0% by weight formalin (30%) 0.1-0.5 wt% polysaccharide Residual water

Another preferred embodiment includes the following Components:

20-30% by weight pendimethalin 15-25 wt% cyanazine 2-10% by weight monoethylene glycol 4-10 wt% emulsifier 0.2-1% by weight of anti-foaming agent 0.1-1% by weight formalin (30%) 0.1-0.5 wt% polysaccharide Residual water

The following example describes a particularly preferred one Embodiment of the invention.

1767 l water, 203.5 kg monoethylene glycol and 407 kg soprophor FL emulsifier (triethanolamine salts of a mixture of phosphoric acid mono- and diesters of a tristyrylphenol polyglycol ether with 18 ethylene oxide units) are placed in a dissolver and with a peripheral speed of 19 to 21 m / sec touched.

Then 1019 kg of atrazine are added over a period of time from 1 to 2 hours at the peripheral speed indicated above dispersed and in circulation with a tooth colloid mill pre-reduced.  

Then the atrazine suspension with external cooling further crushed by the tooth colloid mill.

This is followed by a further grinding process using a Pearl mill, which is repeated depending on the grain size. The Suspension strongly cooled and after grinding in a cooled Pumped dissolver.

At a temperature in the range of 5 to a maximum of 10 ° C, the melted Pendimethalin sprayed into the atrazine suspension.

The suspension obtained is again in the tooth colloid mill ground to further crush the particles. That close grinding processes in the tooth colloid mill again and in the pearl mill. The milling processes in the pearl mill are repeated as necessary, each time with good cooling is respected. The throughput through the pearl mill is approximately 2000 l / h and the outlet temperature of the material from the mill is a maximum of 16 ° C.

As soon as a sufficient degree of fineness is reached, the Suspension is pumped into a cooled dissolver via a cooler. Then it is at a peripheral speed of about 10 m / sec stirred and over 24 hours with a thickener solution from 10.45 kg formalin, 10.45 kg Rhodopol 23 and 512 l water transferred. The peripheral speed is briefly increased to 21 m / sec increased and then set to 5 m / sec. Subsequently is stirred for 1 hour and the suspension with 5.3 kg of anti-foaming agent transferred and degassed.

A milky-yellow suspension is obtained as the end product.

The particle size distribution of the suspended particles in the end product is using a disc centrifuge (sedimentation measurement) determined. 100% <10 µ and 95% <8 µ apply.

Claims (8)

1. Liquid pesticides in the form of an aqueous dispersion which contains one or more active ingredients melting below 70 ° C and one or more active ingredients melting above 70 ° C, characterized in that the active ingredients melting below 70 ° C as a dispersion in Water in combination with an aqueous suspension concentrate of the active ingredients melting above 70 ° C. are present. 2. Liquid pesticidal agent according to claim 1, characterized characterized in that the below 70 ° C melting active ingredient from the Group of trifluralin, pendimethalin, dinoseb acetate, Diclofopmethyl, pyrazophos and (4-amino-3,5-dichloro- 6-fluoro-2-pyridine) oxylacetic acid isooctyl ester selected is and the active ingredient melting above 70 ° C from the group of endosulfan, diuron, atrazine, cyanazine, Simazin, isoproturon, linuron, captafol, carbendazim or fentin hydroxide is selected.   3. Liquid pesticides according to claim 1 and 2, characterized in that it is also a dispersant and / or a wetting agent and optionally further additives and / or Contains aids. 4. Liquid pesticides according to claim 1 to 3, characterized in that it 5 to 50 wt .-% of melting below 70 ° C. Active ingredient and 5 to 50 wt .-% of above 70 ° C. melting active ingredient and 2 to 20 wt .-% emulsifier and in each case less than 1% by weight of defoaming agent, formalin and contains polysaccharide. 5. Liquid pesticides according to claim 1 to 4, characterized in that the active ingredient concentrate as emulsifiers triethanolamine salts a mixture of phosphoric acid mono- and diesters a tristyrylphenol polyglycol ether with 18 EO units, Amine salts of ethoxylated polyacrylphenols, polyglycol ethers of a phenol aldehyde, condensation products of Alkylphenols with formaldehyde and polyamines or a Mixture of ionic and non-ionic surfactants contains. 6. Liquid pesticides according to at least one of the claims 1 to 5, characterized by a Content of 20-30% by weight pendimethalin 15-25% by weight atrazine 2-5% by weight monoethylene glycol 5-10% by weight emulsifier 0.2-1.0% by weight of anti-foaming agent 0.1-0.5% by weight formalin (30%) 0.1-0.5 wt% polysaccharide Residual water   7. Use of the agent according to claims 1 to 6 for crop protection. 8. Process for producing a liquid pesticide Agent according to one of claims 1 to 6, characterized characterized in that at known way of melting at a higher temperature Active ingredient presented in water and auxiliaries and is dispersed and in a further process step the one melting at a lower temperature Active ingredient in molten form injected into the suspension becomes.