The method of obtaining alkali salts of n- (heterocyclizations)arylsulfonamides in the form of water-soluble granules
(57) Abstract:Describes how to obtain the alkaline salts of N-(heterocyclizations)arylsulfonamides formula I , where R1-Cl COOCH3; R2-CH3, OCH3; R3-CH3; X=N, CH; M is Na, K in the form of water-soluble granules by the interaction of equimolar amounts of the corresponding N-(heterocyclizations)-arylsulfonamides IV and hydroxide of an alkali metal and granulating the obtained salts, characterized in that the obtaining of salt, its crystallization and granulation is carried out in one apparatus in the fluidized bed by a continuous supply of dispersed aqueous solution of the hydroxide of an alkali metal concentration of not less than 35%, preferably 40 to 44%, the layer of solid particles consisting of compounds IV and I with the addition of surfactants, moving with a speed of 8 to 11 m/s, and the process is conducted at 20-40oC and humidity not more than 14%, preferably 8-12%. The technical result - obtaining the target product that meets the customer's requirements. The invention relates to a method for producing sodium and potassium salts of N-heterocyclization/arylsulfonamides General formula
< / BR>where R1- Cl COOCH
< / BR>where R1, R2, R3, X, and M have the above meanings /U.S. patent N 4127405 and EPO patent N 559044/.In laboratory conditions, it is relatively easy to get this reaction a small amount of salt satisfactory quality. Sulfonylureas IV not dissolve in water, so the reaction is usually carried out in aqueous-alcoholic medium.In an industrial environment using machines reactor type. The obtained Sol vykristallizovyvalas, filtered and dried, then from preparing preparative form, which also represents Mnogotochie its regeneration, create systems to capture and ensure the explosion.The obtained salt is quickly compressed, which creates further problems when it is used for making the preparative form. The experiments showed the unsuitability of this method of obtaining salt I in pilot conditions.In accordance with the present invention the problem was solved by carrying out the process of obtaining salts of formula I, and at the same time the crystallization and granulation in the fluidized bed, as well as by determination of technological parameters, the combination of which allows to carry out the process and get products that meet customer requirements, and is suitable for use for the above purpose.The known process of obtaining granulated formulations of N-/heterocyclization/ arylsulfonamides in the fluidized bed through the water on a moving layer of material from the pre-pulverized mixture of ingredients, including the active substance, surface-active agent and an inert carrier /see U.S. Pat. USA N 4127405, page 23/.The special feature of this process is that when the contact dispergirovannogo mainly crystallization rate. The chemical reaction of the salt, its crystallization and the formation of granules.For the implementation process of the proposed method the dispersed solution of alkali concentration of at least 35%, preferably 40 to 44%, is continuously applied to the layer of solid particles consisting of sulfonylureas IV and salt I with the addition of surfactants and moving with the speed of 3-11 m/s, which creates a rotating device. The temperature must be maintained in the range of 20 - 40oC and humidity not higher than 14%, preferably 8-12%.Only subject to all conditions stated above provided the maximum gross surface of contact between the solid and liquid phases required to complete the course of chemical reactions and optimal heat exchange, and exclude such phenomena as the channel translating, aggregation, and mainly the possibility of decomposition thermostabilised target products.The proposed method has a simple process design, process of formation of the salt, its crystallization and granulation is carried out in one apparatus. However, due to the absence of dust particles and explosive products is not required topolnica the quality of drugs in content of the active substance, and granulometric composition and the form of granules. The products have good appearance, easy to use, are good for storage.The obtained water-soluble granules can be used for preparation of solutions, as well as directly by embedding in the soil or processing plants.The following are examples of implementation of the method.Example 1. Obtaining potassium salt of chlorsulfuron.In the apparatus with a capacity of 7 liters with a shirt that moves water, and a mixing device on the underlayer particles chlorsulfuron and reture of its potassium salt and sodium lignosulphonate, moving with a speed of 10 to 11 m/sec, serves a 43% solution of potassium hydroxide in dispergirovannom the state in the amount of 0.6 kg/HR humidity of the reaction mass to 8%, temperature 20 - 30oC.The time of crystallization of salt for 10 minutes. At the end of the process, the granules are dried by filing a shirt in hot water. Potassium salt of chlorsulfuron is obtained with a quantitative yield in the form of granules rounded. The content of active substance 92%, surfactant 4%. Particle size: less than 0.2 mm - 5%
0,2 - 1,5 mm - 80%
more than 1.5 mm to 15%.
oC.The time of crystallization of salt 12 minutes. The obtained granulate is dried by filing a shirt in hot water. Sodium salt of chlorsulfuron is obtained with a quantitative yield in the form of granules, rounded forms of the following composition: less than 0.2 mm - 7%; 0,2 - 2 mm - 75%; more than 2 mm to 18%.The content of active substance 94%, surfactant 2%.Example 3. Obtaining potassium salt of sulfometuron.In the apparatus with a capacity of 7 liters with a shirt that moves water, and a mixing device on the sublayer sulfometuron, retur its potassium salt and surfactant /sulfite-yeast brew, SBD/ moving with the speed of 9-11 m/sec., served 43% solution of potassium hydroxide in dispergirovannom the state in the amount of 0.4 kg/h, temperature 20 - 30oC, humidity 12%. The time of crystallization of salt for 20 minutes. The granulate is dried by hot water in the jacket. Output K2 mm - 18%. The performance was 1 kg/h.Example 4. Obtaining the sodium salt of sulfometuron.In the apparatus with a capacity of 7 liters with a shirt that moves water, and a mixing device on the sublayer sulfometuron, retur its sodium salt, and surfactant /Las sodium/ moving with the speed of 6-9 m/sec., serves 35% solution of sodium hydroxide in dispergirovannom the state in the amount of 0.5 kg/h, temperature 20 - 30oC, humidity 8%. The time of crystallization of salt 20 minutes Granulate is dried by hot water in the jacket.Get with a quantitative yield of product in the form of rounded granules of the following composition: less than 0.2 mm - 16%, 0,2 - 2 mm - 75%, more than 2 mm to 9%. The content of active substance - 93%, surfactant - 4%. The method of obtaining alkali salts of N-(heterocyclizations)arylsulfonamides formula I
< / BR>< / BR>where R1- CI, SOON3;
R2- CH3, OCH3;
X IS N, CH;
M - PA, TO,
in the form of water-soluble granules by the interaction of equimolar amounts of the corresponding N-(heterocyclizations)arylsulfonamides formula IV
and hydroxide of an alkali metal and granulation floor is pirate in the fluidized bed by a continuous supply of dispersed aqueous solution of the hydroxide of an alkali metal concentration of not less than 35%, preferably 40 to 44%, the layer of solid particles consisting of compounds IV and I with the addition of surfactants, moving with a speed of 3 -- 11 m/s, and the process is conducted at 20 to 40oC and humidity not more than 14%, preferably 8 to 12%.
< / BR>where R1= Cl, COOCH3;
R3= CH3, ON=C(CH3)2, ON=C(CH3)C2H5;
R4= H, CH3,
used in agriculture as herbicides and plant growth regulators
< / BR>The invention relates also to a method of controlling undesirable vegetation in crops of flax by processing plants weed-killing drug on the basis of salts of formula I, as well as its mixture with other herbicide-active compounds, for example with dimethylamine salt of 2-methyl-4-chlorophenoxyacetic acid
< / BR>and it acceptable in agriculture salts, hydrates and complexes with lower alcohols
and ammonium salts of 2-methoxy-3,6-dichlorobenzoyl acid(dicamba) formula
R1- CH3or C2H5;
R2- H or CH2CH2OH
FIELD: organic chemistry, herbicides, agriculture.
SUBSTANCE: invention describes a synergistic composition of herbicides comprising components (A) and (B) wherein (A) represents herbicide taken among the group of the formula (I):
wherein R1 means (C1-C4)-alkyl; R2 means (C1-C4)-alkyl; R3 means hydrogen atom; X and Y mean (C1-C4)-alkoxy-group; (B) represents one or two herbicides taken among the group of compounds or their acceptable forms: alachlor, metolachlor, acetochlor, dimetenamide, atrazine, cyanasin, metribusin, fluthiamide, nicosulfuron, rimsulfuron, primisulfuron, pendimetalin, sulcotrion, dicamba, mesotrion, isoxachlortol, metosulam, anilofos, fenoxaprop-ethyl, setoxydim, diclofop-methyl, MCPA, bromoxynil, pyridat, clopyralid, iodosulfuron-methyl, ethoxysulfuron, amidosulfuron, gluphosinat-amminium, isopropylammonium-glyphosate, imasetapir wherein components (A) and (B) are taken in the effective doses. Also, invention describes a method for control of weeds by using above indicated herbicide composition. Invention provides the development of the synergistic herbicide composition eliciting high activity.
EFFECT: improved method for control, valuable properties of composition.
6 cl, 26 tbl, 3 ex
FIELD: organic chemistry, agriculture.
SUBSTANCE: claimed mixture from herbicides and antidotes contains (A) herbicidically active substance based on phenylsulfonylureas of formula I and salts thereof (in formula R1 is hydrogen or C1-C6-alkyl; R2 is C1-C3-alkyl; R3 is C1-C3-alkoxy; R4 is hydrogen or C1-C4-alkyl; Hal is fluorine, chlorine, bromine, or iodine); and (B) antidote of formulae II or III , wherein X is hydrogen, halogen, C1-C4-alkyl; C1-C4-alkoxy, nitro or C1-C4-haloalkyl; Z is hydroxyl, C1-C8-alkoxy, C3-C6-cycloalkoxy, C2-C8-alkenyloxy, C2-C8-alkynyloxy; R5 is C1-C2-alkandiyl chain optionally substituted with one or two C1-C4 alkyl residues or (C1-C3-alcoxy)carbonyl; W is bivalent heterocyclic residue; n = 1-5; in weight ratio herbicide/antidote of 100:1-1:100. Also disclosed is method for protection of cultural plants against phytotoxic side effect of herbicidically active substance of formula I. Claimed method includes antidote application of formulae II or III on plant, plant parts, plant seeds or seeding areas before or together with herbicidically active substance in amount of 0.005-0.5 kg/hectare in weight ratio of 100:1-1:100.
EFFECT: mixture for effective selective weed controlling in cultural plant, particularly in maize and grain cultures.
8 cl, 2 ex, 7 tbl