Method of obtaining alkali metal salts of n-phosphonomethylglycine |
|
|
IPC classes for russian patent Method of obtaining alkali metal salts of n-phosphonomethylglycine (RU 2364601):
Method of obtaining ethylenediammonium bis(1-hydroxyethane-1,1-diphosphonato(2-))cuprate(+2), zincate(+2) and nickelate(+2) / 2352575
Invention relates to obtaining etyheleneammonium bis(1-hydroxyethane-1,1-diphosphonato(2-))cuprate (+2), etyheleneammonium bis(1-hydroxyethane-1,1-diphosphonato(2-)) zincate(+2) and etyheleneammonium bis(1-hydroxyethane-1,1-diphosphonato(2-)) nickelate(+2) and can be used for processing toxic wastes of obtaining metal coatings - waste electrolytes of galvanic copper, zinc and nickel plating, waste solutions of chemical nickel plating and copper plating. Products, obtained by said method, can be used for preparation of electrolytes, metal corrosion inhibitors, for obtaining various copper, zinc and nickel compounds, including catalysts of organic and inorganic substance synthesis. Claimed method includes using liquid industrial wastes, containing metal(+2), ethyleneammonium and/or anion of 1-hydroxyethane-1,1-diphosphonic acid as reagents. Target products are obtained by crystallisation from reaction water solution with separation of sediment from solution, process is carried out at temperature from (-5) to 105°C and atmospheric pressure. Method allows to obtain pure crystalline products with yield up to 98%, to reduce expenditures on environment protection.
 Chemical compounds, pharmaceutical cmposition, containing them, their application (versions) and method of binding erα and erβ -estrogen receptors / 2352555
Invention relates to novel compounds of formula (I), including its pharmaceutically acceptable salts, solvates, ethers and amides, possessing ability to bind ERα- and ERβ-estrogen receptors, to pharmaceutical composition based on them, to versions of applying claimed compounds in medication preparation and to method of binding ERα- and ERβ-estrogen receptors.
 Complexonate nitrylotri(methylenphosphonat)-2-phenyl-3-ethyl-8-oxychinolin sodium salts salt-deposition inhibitor / 2337915
Invention relates to novel chemical compounds as salt-deposition inhibitors and can be used in oil industry in oil extraction, in particular in system of sewage water utilising, as well as in systems of circulating water supply of industrial enterprises. Suggested is complexonate of nitrylotri(methylenephosphonato)-2-phenyl-3-ethyl-8-oxychinolin sodium salt of formula
 Long-chain alkylphosphonic acids as soft steel corrosion inhibitors and their production / 2337914
Invention relates to phosphoroorganic chemistry, namely, to method of obtaining long-chain alkylphosphonic acids, possessing anticorrosion activity, based on α-olefins of industrial fraction C16-C18 and C20-C26. Invention can be applied for protection of pipelines, reservoirs, construction metallic structures, equipment for extraction, transportation and processing oil and gas, in metal processing. Long-chain alkylphosphonic acids are obtained by interaction of α-olefins of industrial fraction C16-C18 and C20-C26 with O,O-dimethylphosphorous acid in molar ratio 1:(1.0-2.0) in presence of benzoyl peroxide in amount of 1.0-5.0% of weight of dimethylphosphorous acid at 110-150°C during 10-12 hours in absence of solvent with further hydrolysis of intermediate higher O,O-dimethyl(alkyl) phosphonates with hydrochloric acid with heating, obtaining target product which represents mixture of long-chain alkylphosphonic acids.
 Amorphous alendronate monosodium, methods of production, based pharmaceutical composition and method of inhibition of bone resobrtion / 2334751
Invention refers to method of production of amorphous alendronate monosodium and to solid pharmaceutical composition having property to invoke bone bulk expansion and containing therapeutically effective amount of amorphous alendronate monosodium, produced by stated method. Method of production of amorphous alendronate monosodium includes solvent removal from alendronate monosodium solution using spray drying.
 Acidic phosphorous containing complex forming reagent and method of obtaining it (versions) / 2331651
The invention pertains to an acidic phosphorous containing reagent, is used in the oil industry, heat energy, textile industry, production of mineral fertilizers and household chemistry, and to methods of obtaining the reagent. The reagent (conventional name "АФК-1") contains the following in given mass %: acetoxyethylidenediphosphonic acid 50.0-95.0 mass %, acetic acid - 29.5-0.5 mass %, the rest is acetic anhydride to 100. The quantitative composition of the indicated reagent is determined by the method of obtaining it and the ratios of the initial reagents. The method of obtaining the reagent involves adding acetic anhydride to a suspension of acetic and phosphorous acid at temperature of 60-90°C for a period of 1.5 hours. The reaction mixture is kept at 100-110°C for 1 hour and acidic impurities are distilled off to a controlled volume of distillate. Similar methods are developed based on phosphorous containing wastes from production of acid chlorides of higher fatty acids. The wastes are treated with water or a water solution of acetic acid with subsequent separation of the organic layer of fatty acids, after which the residue, containing phosphorous acid, is treated with phosphorous tri-chloride and acetic anhydride at 115-130°C, and acidic impurities are distilled off to the controlled distillate volume.
 Acidic phosphorous containing complex-forming reagent and method of obtaining it / 2331650
Invention pertains to the chemistry of phosphorous organic compounds, and specifically to an acidic phosphorous containing complex-forming reagent, which can be used in the oil industry, heat energy, textile industry, production of mineral fertilizers and household chemistry, and to the method of obtaining it. The acidic phosphorous containing complex-forming reagent (conventional name "АФК-2") contains the following in mass %: acetoxyethylidenediphosphonic acid - 50-95 mass %, acetic acid - 50-5 mass %. The method of obtaining the composition involves adding phosphorous tri-chloride, acetic acid and water simultaneously to glacial acetic acid in molar ratios equal to 1:(4.5-5.5):(1.93-1.95), at temperature of 35-45°C with subsequent keeping of the reaction mixture at 110-120°C for a period of 2 hours and controlled distillation of acidic impurities to the required distillate volume.
Method of obtaining inhibitor of precipitation of mineral salts / 2329270
Invention pertains to the method of obtaining an inhibitor of precipitation of mineral salts, The inhibitor is obtained by reaction of hexamethylenediamine and ammonium chloride with formaldehyde and phosphorous acid in a medium of diluted hydrochloric acid at high temperature with subsequent neutralisation of the obtained solution using sodium hydroxide to pH of 6.5±1.0. The process is carried out with molar ratio of hexamethylenediamine to ammonium chloride of 1:3-6.
 Plasma carboxypeptidase b inhibitors / 2323223
Invention describes compound of the formula (I):
 Method for preparing monohydroperfluoroalkanes, bis-(perfluoroalkyl)phosphinates and perfluoroalkylphosphonates / 2319705
Invention describes a method for synthesis of monohydroperfluoroalkanes, bis-(perfluoroalkyl)phosphinates and perfluoroalkylphosphonates. Method involves treatment of at least one perfluoroalkylphosphorane with at least one base wherein base(s) are chosen from group consisting of alkali-earth metal hydroxides, metalloorganic compound in useful solvent or at least one organic base and an acid in useful reaction medium. Also, invention describes novel perfluoroalkylphosphonates and bis-(perfluoroalkyl)phosphinates, using novel perfluoroalkylphosphonates and bis-(perfluoroalyl)phosphinates as ionic liquids, catalysts of phase transfer or surfactants.
 Phosphonate derivatives / 2258707
Invention relates to new biologically active phosphonate compounds. Invention describes phosphonate compound of the formula:
 Method for preparing n-phosphonomethylglycine and intermediate substance for its preparing / 2260010
Invention relates to the improved method for preparing N-phosphonomethylglycine. Method involves interaction of derivative of hexahydrotriazine of the formula (II):
Chloride removing in method for preparing phosphonomethyliminodiacetic acid / 2263116
Invention relates to a selective method for removing chloride as NaCl from waste in method for preparing N-phosphonomethyliminodiacetic acid. The waste flow is neutralized with NaOH to pH value about 7, water is evaporated from flow of neutralized waste under atmospheric or lower pressure at temperature from 40°C to 130°C until to precipitation of NaCl. The precipitate is filtered off at temperature from 35°C to 110°C to isolate NaCl from filtrate and NaCl is washed out with saturated saline solution. Invention provides effective removal of NaCl from waste in a method for manufacturing N-phoaphonomethyliminodiacetic acid.
 New acyclic nucleoside phosphonate derivatives, their salts and method for preparing these compounds / 2266294
Invention relates to acyclic nucleoside phosphonate derivatives of the formula (1):
 Method for preparing nickel (ii) bis-(1-hydroxyethane-1,1-diphosphonate (1-)) / 2271362
Method involves preparing nickel (II) bis-(1-hydroxyethane-1,1-diphosphonate (1-)) by addition 1-hydroxyethane-1,1-diphosphonic acid in the concentration 0.2-4.5 mole/l to an aqueous solution containing nickel (II) in the concentration 0.1-2.0 mole/l and organic solvent mixing with water followed by crystallization of the end substance from the solution. Method provides preparing the pure homogeneous end product with high yield, and utilization of depleted electrolyte in nickel plating representing a toxic waste in galvanic manufacture.
 Method for preparing n-phosphonomethylglycine / 2274641
Invention relates to a method for preparing N-phosphonomethylglycine. Invention describes a method for preparing N-phosphonomethylglycine from an aqueous mixture containing dissolved N-phosphonomethylglycine, ammonium halides, alkali or earth-alkali metal halides and, optionally, organic impurities. Method involves (a) using a mixture with pH value from 2 to 8; (b) separation of mixture is carried out on a selective nanofiltration membrane, and retentate enriched with N-phosphonomethylglycine and depleted with halides and permeate depleted with N-phosphonomethylglycine are obtained, and (c) N-phosphonomethylglycine is isolated from retentate. Method provides preparing N-phosphonomethylglycine in simultaneous separation of halide salts.
Method for preparing copper (ii) bis-(1-hydroxyethane-1,1-diphosphonate (1-)) from production waste / 2280647
Invention relates to technology of organic substances, in particular, to the improved method for preparing copper (II) bis-(1-hydroxyethane-1,1-diphosphonate (1-)). The final copper (II) bis-(1-hydroxyethane-1,1-diphosphonate (1-)) is prepared by crystallization from aqueous solution with concentrations of copper salt (II) from 0.5 to 2.0 mole/l and 1-hydroxyethane-1,1-diphosphonic acid with concentration from 2.0 to 6.0 mole/l prepared by using copper-containing waste in galvanic and electronic engineering manufacture, or by using a semi-finished product from production of 1-hydroxyethane-1,1-diphosphonic acid. Invention provides reducing cost in production of copper (I) bis-(1-hydroxyethane-1,1-diphosphonate (1-)) in combination with retaining purity, expanded raw base for preparing the end product and utilization of manufacture waste.
 Stimulator of growth agricultural root crop plants / 2283317
Invention describes bis-(diethylammonium)-dihydrogen-1-hydroxyethyl-1,1diphosphonate monohydrate of the formula (I)
 Method for preparing bis-(1-hydroxyethane-1,1-diphosphonate(1-)) zinc (ii) / 2287532
Invention relates to the improved method for preparing bis-(1-hydroxyethane-1,1-diphosphonate(1-)) zinc (II). Method involves interaction of zinc-containing reagent and 1-hydroxyethane-1,1-diphosphonic acid in a solvent medium, crystallization of the end product from solution, separation of deposit from solution and drying the deposit. Method involves using water-soluble zinc (II) salt with anion of strong acid as a zinc-containing reagent and preparing the solution with the concentration of zinc (II) salt from 0.2 to 2.2 mole/l and the concentration of 1-hydroxyethane-1,1-diphosphonic acid from 0.4 to 5.0 mole/l. The end product prepared by proposed method can be used in preparing phosphonate electrolytes for galvanic zinc-plating, for preparing zinc-phosphate inhibitors of steel corrosion, as trace supplement to vitamin preparations and fodders for animals, as a zinc microfertilizer in agriculture and for preparing other compounds of zinc (II). Invention provides enhancing purity and uniformity of the end product, increasing its yield, improved technological effectiveness of process, utilizing toxic waste in galvanic manufacturing.
Method for preparing crystalline nitrilotrimethylphosphonic acid disodium salt monohydrate / 2293087
Invention relates to technology for synthesis of crystalline nitrilotrimethylphosphonic acid sodium salts. For synthesis of nitrilotrimethylphosphonic acid disodium salt monohydrate the method involves preliminary synthesis of nitrilotrimethylphosphonic acid by interaction of phosphorus trichloride, formaldehyde and ammonia or its derivative followed by neutralization with sodium hydroxide in the content in the reaction mass 46-54 wt.-% of nitrilotrimethylphosphonic acid and 6.0-16.0 wt.-% of hydrogen chloride up to pH value 2.5-4.5, and isolation of the end compound by crystallization. The mass part of the main substance in synthesized product is 88-95%, the content of chloride ions is 1.2-2.0%, yield is 50-60% as measured for PCl3. Synthesized compound is recommended for using as chelate compounds as a component of detergents, anti-rheological additive in drilling solutions, plasticizing agents for building concretes, in wine-making industry, as inhibitors of salt depositions in heat and power engineering and others fields.
|
FIELD: chemistry. SUBSTANCE: claimed invention relates to method of obtaining alkali metal salts of N-phosphomethylglycine and can be applied in agriculture, for fight against weeds. Claimed method lies in the following: reaction of glyphosate and alkaline reagent interaction is carried out in solid phase in highly efficient mixer in conditions of crashing and in close contact of reaction components. EFFECT: development of new method for obtaining N-phosphomethylglucine salts without solvents. 4 cl, 4 ex
This invention relates to the petrochemical industry, and more specifically, to obtain alkali metal salts of organic acids, which are used in pure form or as intermediates in the production of economic goods. So, alkali metal salts of biologically active organic acids are used as herbicide funds in the fight against weeds ("Handbook of pesticides and agrochemicals permitted for use on the territory of the Russian Federation", Moscow, 2007, publishing house "Agrorus", str, 177). In this invention we are talking about a method of producing alkali metal salts of N-phosphonomethylglycine (glyphosate) as a herbicide funds for destruction of weeds ("Handbook of pesticides and agrochemicals permitted for use on the territory of the Russian Federation", Moscow, 2007, publishing house "Agrorus", str). Known conventional option of obtaining alkali metal salts of organic acids, when an aqueous solution of the alkaline agent is in contact with an organic acid. For example, in U.S. Pat. U.S. No. 6096686 potassium salt of N-phosphonomethylglycine (glyphosate) is obtained by neutralization of the glyphosate aqueous solution of KOH to a pH equal to 7. However, as is common variant of the synthesis of alkaline salts of organic acids, and specifically potassium salt GL is fosatu have fault, associated with significant costs if you need to get dry (anhydrous) salts, namely the introduction of additional process steps, including evaporation, unloading and drying salt. Getting dry (anhydrous) alkali metal salts of glyphosate opens the prospect of creating a new glyphosate containing products in the form of water-soluble powders or water-soluble granules. New progressive forms allow you to raise the concentration of biologically active agent (glyphosate) in the product up to 700 g or more per 1 kg and significantly impact on the economy of the production of glyphosate containing products. The present invention is to develop a method of producing alkali metal salts of glyphosate in a dry (anhydrous) variant that eliminates the shortcomings of traditional methods of obtaining such salts. This object is achieved in that the formation of alkali metal salts of glyphosate is carried out in a solid phase under conditions of mechano-chemical interaction of glyphosate and an alkaline reagent (NaOH, KOH, N2CO3To2CO3with Tonino grinding no more than 20 microns in effective Z-shaped worm-blade mixer, ensuring close contact of the components of the reaction. To implement the invention can be used l the all other mechanical devices, providing functions of crushing and contact the solid reactants. It can be electromagnetic shredders, high-speed multi-blade centrifugal mixers, etc. Experiments were performed as follows. In the Z-shaped mixer downloaded the estimated amount of the powder of glyphosate and an alkaline reagent (NaOH, KOH, N2CO3To2CO3with Tonino grinding no more than 20 microns, included mixer (rotation rate of the mixing device 60 rpm) at ambient temperature. The reaction time varied from 60 to 90 minutes Transition of crystalline structures of glyphosate and an alkaline reagent in solid crystalline alkali salt of glyphosate is on the middle of the reaction through a stage of powdery amorphous state. Upon completion of the reaction from the mixer get dry, loose corresponding salt of an alkali metal glyphosate, in the case of alkali and without the stage of formation of the amorphous state due to the selection process of the reaction of carbon dioxide, in the case of carbonates. Two of the considered structures of alkaline chemicals (alkalis and carbonates) should be preferred carbonates, because they, unlike pure alkali, leave in the reaction products two times less water of crystallization (4.3% as against 8.6 per cent for alkalis). Output about what aktov reaction was determined as the ratio of the weight actually unloaded the reaction products together with crystallization water to theoretically calculated. The above is illustrated by the following examples. Example 1 In the Z-shaped mixer was downloaded 169 g (1 mol) of powdery glyphosate and 40 g (1 mol) of powdered NaOH. When the ambient temperature was performed solid-phase reaction for 70 min Uploaded 204,9 g dry powdered Na-salt of glyphosate. The estimated weight of Na-salt of glyphosate according to the reaction 209, the Output of the Na-salt of glyphosate 98%. Example 2 Analogously to example 1 was downloaded 169 g (1 mol) of glyphosate and 56 g (1 mol) of KOH. The reaction time of 60 minutes was Unloaded to 220.3 g (225 g estimated number) dry powder K-salt of glyphosate. Access To the salt of glyphosate is 97.7%. Example 3 Analogously to example 1 was downloaded 169 g (1 mol) of glyphosate and 53 g (0.5 mol) of Na2CO3. Carried out the reaction for 90 min Uploaded 195,4 g (200 g estimated number) of dry powdered Na-salt of glyphosate. The output of the Na-salt of glyphosate, which is 97.5%. Example 4 Analogously to example 1 was downloaded 169 g (1 mol) of glyphosate and 69 g (0.5 mol)2CO3. Carried out the reaction within 80 minutes Unloaded 210,5 g (216 g estimated number) dry powder K-salt of glyphosate. The output of the K-salt of glyphosate 97,4%. 1. The method of obtaining alkali metal salts of N-phosphonomethylglycine (glyphosate), characterized in that the reaction of interaction of glyphosate and the alkaline reagent is carried out in the solid phase in high-performance is Musicale in conditions of grinding and closely components of the reaction. 2. The method according to claim 1, characterized in that the crushing of the components of the reaction should be not more than 20 μm. 3. The method according to claim 1, characterized in that the reaction of the interaction is carried out at ambient temperature. 4. The method according to any one of claims 1 to 3, characterized in that the interaction time is 60-90 minutes
|