CS270504B1 - Suspension concentrate of abrasive - Google Patents

Suspension concentrate of abrasive Download PDF

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CS270504B1
CS270504B1 CS863786A CS378686A CS270504B1 CS 270504 B1 CS270504 B1 CS 270504B1 CS 863786 A CS863786 A CS 863786A CS 378686 A CS378686 A CS 378686A CS 270504 B1 CS270504 B1 CS 270504B1
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Czechoslovakia
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atrazine
suspension concentrate
isopropylamino
ethylamino
chloro
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CS863786A
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Czech (cs)
Slovak (sk)
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CS378686A1 (en
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Robert Ing Csc Poor
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Poor Robert
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Abstract

Riešenie ša týká suspenzného koncentrátu atrazínu, ktorý obsahuje 40 až 55 % hmot. 2-izopropylamíno-4-etylamíno-6-chlór-s-triaz£nu technického o čistotě 92 až 98 %, 2 až 10 % hmot. monoetylénglykolu, 0,5 až 5 % hmot. zmesi anion- a kationaktívnych látok, ktgrých viskozita pri 25 °C je 150 až 250 m.Pa.s, 0,1 až 0,015 % hmot. polysacharidu na báze mikroorganizmov radu .Xanthomonas a 25 až 40 % hmot. vody. Prípravok, ktorý sa využívá v polnohospodárstve ako herbicid, sa vyznačuje vysokou stabilitou pri skladovaní .The solution relates to a suspension concentrate of atrazine which it contains 40 to 55 wt. 2-isopropylamino-4-ethylamino-6-chloro-s-triazine technical purity 92 to 98% 2 to 10 wt. monoethylene glycol, 0.5 to 5 wt. anionic and cationic mixtures substances the viscosity at 25 ° C is 150 to 250 m.Pa.s, 0.1 to 0.015 wt. polysaccharide based microorganisms of the .Xanthomonas series and 25 to 40 wt. water. The product that is uses as a herbicide in agriculture, is characterized by high storage stability .

Description

Vynálezom je suspenzný koncentrát 2-izopropylamíno-4-etylamíno-6~chlór-s-triazínu obsahujúci až 55 % hmotnostných účinnej látky atrazínu.The invention is a suspension concentrate of 2-isopropylamino-4-ethylamino-6-chloro-s-triazine containing up to 55% by weight of the active ingredient atrazine.

Medzi najznámejšie a najviac vyrábané s-triazínové herbicidy patří 2-izopropylamíno-3-etylamíno-5-chlór-s.-triazín (atrazín). Herbicídne účinky bolí objavené v roku 1954 vo Svajčiarsku a sú popísáné vo švajčiarskom patente 229 227. Příprava atrazínu reakciou kyanurchloridu, etylamínu, izopropylaminu a hydroxidu sodného vo vodnochlórbenzénovom prostředí je popísaná v Československem patente 110 352.Příprava atrazínu reakciou kyanurchloridu a etylamínu, izopropylamínu v prostředí bezvedného organického rozpúštadla, pričom na viazanie vzniklého chlorovodíka sa použije bezvodného amoniaku, popisuje švajčiarsky patent 508 640. Získaný produkt obsahuje 92 % atrazínu. Vplyv hodnoty pH na výtažek atrazínu popisujú patentové spisy NDR a NSR. Podia NDR patentu 51 646 sa najlepší výtažek dosiahne vtedy, ak v prvom reakčnom stupni, t.j. po přidaní prvého aminu a hydroxidu alkalického kovu sa udržuje hodnota pH 6 až 8, v druhem reakčnom stupni, t.j. po přidaní druhého aminu a hydroxidu alkalického kovu, sa udržuje hodnota pH na 8,5 až 9. Výtažok atrazínu je 96 %. V NSR patente 2 032 861 sa udává hodnota pH v prvom stupni 6,5 až 10. V USA patente 3 328 399 a 3 586 679 je popísaný spósob přípravy atrazínu z kyanurchloridu, etylamínu, izopropylamínu v bezvodnom prostředí pri teplote 120 - 170 °C za oddestilovania vzniknutého chlorovodíka. Výhoda sposobu je, že odpadne problém odpadných vod s obsahem minerálnych solí. Vo švajčarskom patente 546 247 sa popisuje adiabatický spásob výroby atrazínu vo vodonerozpustnom rozpúštadle reakciou etylamínu, izopropylamínu, alkalického hydroxidu s kyanurchloridom.Vo francúzskom patente 2 296 628, rumunskom patente 68 016, japonskom patente 131 592 (1977) sa doporučuje pri dávkovaní amínov pri výrobě atrazínu dávkovat prvý izopropylamín. Bank. C. a spol. J. Am. Chem. Soc. 66 1771 (1944) a Pridheim E., J. Am. Chem. Soc. 66 1725 (1944) doporučujú pri prvom reakčnom stupni výroby atrazínu teplotu okolo O °C a druhý reakčný stupeň pri teplotách 30 - 50 °C. Pri prvom reakčnom stupni sa ako reakčné prostredie používá zmes vody a ladu, připadne voda, lad a organické rozpúštadlo.The best known and most widely produced s-triazine herbicides include 2-isopropylamino-3-ethylamino-5-chloro-s.-triazine (atrazine). Herbicidal effects were discovered in 1954 in Switzerland and are described in Swiss patent 229 227. The preparation of atrazine by the reaction of cyanuric chloride, ethylamine, isopropylamine and sodium hydroxide in aqueous chlorobenzene medium is described in Czechoslovak patent 110 352. The preparation of atrazine by the reaction of ethylamloride Anhydrous organic solvent, using anhydrous ammonia to bind the resulting hydrogen chloride, is described in Swiss Patent 508,640. The product obtained contains 92% of atrazine. The effect of pH on atrazine yield is described in the GDR and NSR patents. According to GDR patent 51 646, the best yield is obtained if in the first reaction step, i. after the addition of the first amine and the alkali metal hydroxide, the pH is maintained at 6 to 8, in the second reaction step, i. after the addition of the second amine and the alkali metal hydroxide, the pH is maintained at 8.5 to 9. The yield of atrazine is 96%. U.S. Pat. No. 2,032,861 discloses a pH of 6.5 to 10 in the first stage. U.S. Pat. Nos. 3,328,399 and 3,586,679 describe a process for preparing atrazine from cyanuric chloride, ethylamine, isopropylamine in an anhydrous medium at 120-170 ° C. distilling off the hydrogen chloride formed. The advantage of this method is that the problem of wastewater containing mineral salts is eliminated. Swiss Patent 546,247 describes an adiabatic process for the production of atrazine in a water-insoluble solvent by the reaction of ethylamine, isopropylamine, alkali hydroxide with cyanuric chloride. atrazine dosed with the first isopropylamine. Bank. C. et al. J. Am. Chem. Soc. 66 1771 (1944) and Pridheim E., J. Am. Chem. Soc. 66 1725 (1944) recommend a temperature of about 0 ° C in the first reaction step for the production of atrazine and a temperature of about 30-50 ° C in the second reaction step. In the first reaction step, a mixture of water and ice or water, ice and an organic solvent is used as the reaction medium.

Technická účinná látka 2-izopropylamíno-4-etylamíno-6-chlór-s-triazín sa finalizuje do formy dispergovatelného prášku obsahujúceho 50 % hm. účinnej látky a podia CSAO 237 107 obsahujúceho až 80 % hm. atrazínu v dispergovatelnom prášku.The technical active substance 2-isopropylamino-4-ethylamino-6-chloro-s-triazine is finalized in the form of a dispersible powder containing 50% by weight. active substance and according to CSAO 237 107 containing up to 80 wt. atrazine in a dispersible powder.

Dosial známe a zaužívané sposoby výroby využívajú finalizáciu atrazínu i do formy suspenzného koncentrátu avšak koncentrácia atrazínu nepřevyšuje 40 t hm. v dispergovateínom koncentráte.Previously known and used production methods use the finalization of atrazine in the form of a suspension concentrate, but the concentration of atrazine does not exceed 40 wt. in dispersible concentrate.

Zistili sme, že je možné připravit dispergovatelný koncentrát obsahujúci až 55 % hm. atrazínu,pričom si zachová vysokú suspenznú stálost i stabilitu pri skladovaní. Pre zabezpečenie vysokej kvality výrobku je nutné dodržat zloženie přípravku podlá predmetu vynálezu.We have found that it is possible to prepare a dispersible concentrate containing up to 55% by weight. atrazine, while maintaining high suspension and storage stability. To ensure the high quality of the product, it is necessary to adhere to the composition of the preparation according to the subject of the invention.

Suspenzný koncentrát 2-izopropylamíno-4-etylamíno-6-chlór-s-triazínu obsahuje až 55 % hm. 2-izopropylamíno-4-etylamíno-6-chlór-s-triazínu (atrazín), ktorého čistota je minimálně 92 % hm., spravidla 95 až 98 %. Ďalej suspenzný koncentrát obsahuje 2 - 10 % hm. monoetylénglykolu, 0,5 až 5 % hm. zmesí anion- i kationaktívnych látok (tenzidov), ktorých viskozita pri 25 °C je 150 - 250 m.Pa.s. Súčastou zloženia je i 0,015 až 0,1 % hm. polysacharidu získaného kultiváciou mikroorganizmov radu Xanthomonas a zvyšok do 100 % hm. tvoří voda.The suspension concentrate of 2-isopropylamino-4-ethylamino-6-chloro-s-triazine contains up to 55% by weight. 2-isopropylamino-4-ethylamino-6-chloro-s-triazine (atrazine), the purity of which is at least 92% by weight, generally 95 to 98%. Furthermore, the suspension concentrate contains 2 - 10 wt. monoethylene glycol, 0.5 to 5 wt. mixtures of anionic and cationic substances (surfactants) whose viscosity at 25 ° C is 150 - 250 m.Pa.s. The composition also includes 0.015 to 0.1% by weight. polysaccharide obtained by culturing microorganisms of the order Xanthomonas and the residue up to 100 wt. forms water.

Suspenzný koncentrát uvedeného zloženia pri dosiahnutí vysokej jemnosti účinnej látky tak, že zvyšok na site 0,125 mm je max. 0,1 % hm., sa vyznačuje vysokou stabilitou charakterizovanou suspenznou stálostou 98 %, po jednom týždni pri teplote 50 °C je suspenzná stálost min. 97 % a po jednotýždňovom tropikateste pri teplote 60 °C je suspenzná stálost minimálně 96 %. Viskozita přípravku počiatočná je 1 100 m.Pa.s a po jednotýždennom skladovaní pri 50 až 60 °C je 1 000 m.Pa.s.Suspension concentrate of said composition while achieving a high fineness of the active substance so that the residue on the sieve 0.125 mm is max. 0.1% by weight, is characterized by high stability characterized by suspension stability of 98%, after one week at 50 ° C the suspension stability is min. 97% and after a one-week tropical test at 60 ° C, the suspension stability is at least 96%. The initial viscosity of the preparation is 1,100 m.Pa.s and after one week of storage at 50 to 60 ° C it is 1,000 m.Pa.s.

CS 270 504 BlCS 270 504 Bl

Příklad 1Example 1

Do banky s miešadlom sa vložilo 420 ml vody a za stálého miešania sa přidalo 1,5 g Rhodopolu. Vzniknutý gel sa nechal bobtnat 120 min. Potom sa do banky doplnilo 30 g emulgátora Atlox 4853 B, ktorý představuje tekutinu o viskozite 150 - 250 m.Pa.s. pri teplote 25 °C, pozostávajúcu zo zmesi anionaktívnych a kationaktívnych tenzidov. Roztok sa homogenizoval pri teplote miestnosti cca 30 min. a Sálej sa postupné nadávkovalo 526 g technického atrazínu o čistotě 95,3 % hm., ktorý bol vopred jemne zomletý tak, že zvyšok na site 0,125 mm bol pod 0,1 %. Po dodávkovaní atrazínu sa přidalo 100 g monoetylénglykolu. Ďalej sa produkt homogenizoval a podrobil sa analýze: obsahoval 46,4 % atrazínu, měrná hmotnost 1 136 g/cm3, suspenzná stálost 1 % roztoku bola 98,2 %.420 ml of water were placed in a stirred flask and 1.5 g of Rhodopol was added with stirring. The resulting gel was allowed to swell for 120 min. Then 30 g of Atlox 4853 B emulsifier, which is a liquid with a viscosity of 150-250 m.Pa.s. at 25 ° C, consisting of a mixture of anionic and cationic surfactants. The solution was homogenized at room temperature for about 30 min. and 526 g of technical atrazine with a purity of 95.3% by weight, which had been pre-finely ground so that the residue on the 0.125 mm sieve was below 0.1%, were gradually metered in. After the addition of atrazine, 100 g of monoethylene glycol was added. Next, the product was homogenized and analyzed: it contained 46.4% atrazine, specific gravity 1,136 g / cm 3 , suspension stability of the 1% solution was 98.2%.

Claims (2)

PREDMET V Y N Á L E Z USUBJECT V Y N A L E Z U Suspenzný koncentrát atrazínu vyznačený tým, že obsahujeAtrazine suspension concentrate, characterized in that it contains 40 až 55 % hm. 2-izopropylamíno-4-etylamíno-6-chlór-s-triazínu technického o čistotě 92 až 98 % 2 až 10 % hm. monoetylénglykolu,40 to 55 wt. Of technical grade 2-isopropylamino-4-ethylamino-6-chloro-s-triazine with a purity of 92 to 98% of 2 to 10% by weight. monoethylene glycol, 0,5 až 5 % hm. zmesi anion- a kationaktívnych látok, ktorých viskozita pri 25 °C je 150 až0.5 to 5 wt. mixtures of anionic and cationic substances whose viscosity at 25 ° C is 150 to 250 m.Pa.s.,250 m.Pa.s., 0,1 až 0,015 % hm. polysacharidu na báze mikroorganizmov radu a Xanthomonas0.1 to 0.015 wt. polysaccharide based on the microorganism series and Xanthomonas 25 až 40 % hm. vody.25 to 40 wt. water.
CS863786A 1986-05-23 1986-05-23 Suspension concentrate of abrasive CS270504B1 (en)

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