CS222894B1 - Method of preparing selective herbicides - Google Patents

Abstract

The invention relates to the preparation of a selective herbicidal composition based on 1-phenyl-4-amino-5-chloro-6-pyridazone, characterized in that SiO2, a dry dispersant, and a sulfite extract are added to finely ground 1-phenyl-4-amino-5-chloro-6-pyridazone containing 1-phenyl-5-amino-4-chloro-6-pyridazone with stirring, the mixture of the above substances is then stirred for 5 to 60 minutes, and an aqueous solution of branched alcohol sulfates is then added and the mixture is homogenized with stirring for 5 to 60 minutes.

Description

222894 3

The present invention provides a process for the final treatment of a 1-phenyl-4-amino-5-chloro-6-pyridazine containing 1-phenyl-5-amino-4-chloro-6-pyridazone for selective herbicides. preparation.

According to known methods and the method of manufacture, the selective active ingredient 1-phenyl-4-amino-5-chloro-6-pyridazone is finalized without the presence of 1-phenyl-5-amino-4 -chloro-6-pyridazone.

The disadvantage of the process used is the need to extract the inactive 1-phenyl-5-amino-4-chloro-6-pyridazone isomer from the reaction mixture containing 1-phenyl-4-amino-5-chloro-6-pyridazone.

Extraction of isa yields the active isomer which is finalized after drying and grinding. At the same time, a solution of the inefficient isomer is obtained which is thickened and represents the second unused product of the technology.

We have found that the process of finalizing a 1-phenyl-4-amino-5-chloro-6-pyridazone based herbicidal formulation can also be accomplished by the presence of an inactive isomer, 1-phenyl-4-chloro-5-amino-6- pyridazone, whereby the process of producing a selective herbicidal composition is substantially simplified.

SUMMARY OF THE INVENTION The present invention provides a process for the preparation of a selective herbicidal composition for the 1-phenyl-4-amino-5-chloro-6-pyridazone ibibase, wherein 100 parts by weight of technical grade 1-phenyl-4- amine-5-chloro-6-pyridazone, containing at most 40 parts of 1-phenyl-5-amino-4-chloro-6-pyridazone, add 0.5 to 8.0 parts by weight of SiO 2, followed by a dry dispenser in 3.0 to 14 wt. 6 to 50 parts by weight of the bisulphide extract are then added with stirring, and the mixture is then stirred for 5 to 60 minutes, and further mixed with 1 to 5 parts by weight of a mixture of propylene oxide and ethylene oxide. 0 to 4.0 parts of an aqueous solution of branched alcohols sulfates, ketoalcohols and ether alcohols having a chain length of C8 to C18. The mixture is homogenized with stirring for 5 to 60 minutes. The advantage of the process is that the order of addition of the components is optional, taking into account the weight ratios of the dosed components, preferably adding an aqueous solution of branched-chain sulphate C8 to C18 and the final component of finalization. The condition for the addition of the aqueous sulphate solution is its fine dispersion into the addition mixture. A further advantage of the present invention is that it is possible to prepare the dry dampener and the SiO2 and the sulphate extract prior to finalizing the active ingredients and to add them already mixed to the final active ingredients.

In order to ensure a high fineness of the final composition, fine grinding of the individual components of the finalization is necessary.

The subject matter of the invention illustrates examples of translations that do not exhaust its scope. Example 1

Do laborat. 320 g of technical 1-phenyl-4-amino-5-chloro-6-pyridazone containing 72.3 wt. by the gas chromatography method, which also contained 25.9% by weight of the inactive 1-phenyl-4-chloro-5-amino-6-pyridazone isomer. The finely milled technical 1-phenyl-4-amino-5-chloro-6-pyridazone of the above composition was finely milled, with a net residue of 0.04 mm being 0.3% and the rest of the 0.125 mm mesh 0.02%. 3.2 g of SiO 2 were added after a stirrer stirrer, 20 g of a dry disperser consisting of kaolin and a mixed copolymer of propylene oxide and ethylene oxide in wt. kaolin to mixed copolymer ratio of 5 to 1. After 10 min. 100 g of dried sulphite liquor was added to the mixture. The mixture of these substances was stirred for 5 minutes, and further 5 g of an aqueous solution of the C8 to C18 chain alcohols, keto-alcohols and ether alcohols were added. An aqueous sulfate solution was added as a finely divided aerosol. The mixture of the above compounds was stirred for 30 minutes, and a sample was collected which was analyzed. The content of 1-phenyl-4-amino-5-chloro-6-pyridazone was 51.28% by weight. gas. chromatography. The rest of the sieve 0.04 mm was 0.4%, on the sieve 0.125 the symbol was 0.08%. The stability of 1% suspension was 80.3 ° / o. EXAMPLE 2 In Example 1, the procedure was followed and proceeded as in Example 1, wherein the technical 1-phenyl-4-amino-5-chloro-6-pyridazone was milled together with siloxide prior to filtration, with SiO2 being 1% by weight of the active ingredient. . The following procedure was followed as in Example 1, whereby the individual components of the finalization were mixed in the following mass. ratio. 72% techn. 1-phenyl-4-amino-5-chloro-6-pyridazine, containing 70.9%! 1% SiO2, 5% dry supernatant, 20% sulphite liquor and 2% aqueous sulphate solution were added. The final herbicidal product obtained had the following quality indicators: 1-phenyl-4-amino-5-chloro-6-pyridazone 50.8 wt. established method gas. chromatography, stability of 1% suspension 79.83%, residue on sieve 0.04 mm was 0.3per. and the residue on the 0.125 mm sieve was 0.05 wt%.

The invention can be used to produce a selective herbicidal preparation based on 1-phenyl-4-amino-5-chloro-6-pyridazone.

Claims (1)

222894 Example 3 To lab. the mixer was weighed with 320 g of a finely divided 1-phenyl-4-amino-5-chloro-6-pyridazine containing 93 wt. active substance is determined by gas chromatography. With stirring, 3.4 g of SiO 2 was added and the procedure was followed as in Example 1. Stability of 1 ° / o of the 78.4 ° / o slurry suspension, sieve shock of 0.04 was 0.38% and on the sieve. 0.125bol 0.1%. FORMULATION The method of preparing a selective herbicidal composition on a 1-phenyl-4-a, m-5-chloro-6-pyridazone base is characterized in that up to 100 wt. parts of finely milled technical 1-phenyl-4-amino-5-chloro-6-pyridazone containing a maximum of 40 parts of 1-phenyl-4-chloro-5-amino-6-pyridazone are added to a 0.5 to 1: 1 mixture. 8.0 wt. parts of SiO 2, a dry disperser in an amount of 30 to 14 wt. die-clay, consisting of kaolin and mixed co-polymer of propylene oxide and ethylene oxide. the kaolin to mixed copolymer ratio of 5 to 1, 6 to 50 parts of the sulphite liquor are further added with stirring, then the carbon blacks of said substances are stirred for 5 to 60 minutes, further 1 to 4 parts of an aqueous solution of sulphates of branched alcohols, keto-alcohols and ether to a C18 to C18 chain, the mixture is homogenized with stirring for 5-60 minutes.