Method of preparing aqueous solution of zinc complex of disodium or dipotassium salt of hydroxyethylidenediphosphonic acid |
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IPC classes for russian patent Method of preparing aqueous solution of zinc complex of disodium or dipotassium salt of hydroxyethylidenediphosphonic acid (RU 2391348):
 Ibandronate polymorph b / 2387661
Invention relates to a new crystalline polymorph of 3-(N-methyl-N-pentyl)amino-1-hydroxypropane-1,1-diphosphonic acid monosodium salt monohydrate (Ibandronate) with formula I, which is characterised by x-ray powder diffraction pattern with characteristic peaks at angles 2-theta: 9.7°, 12.2°, 14.4°, 16.8° and 25.8°, IR-spectrum with characteristic peaks, cm-1: 3679, 3164, 2955; 2854, 1377, 1290, 1157, 1093, 1068, 1035, 965, 951, 933, 905, 761 and 723, as well as a vibrational Raman spectrum with characteristic peaks, cm-1: 2968, 2951, 2928, 2887, 2849, 1441, 1308, 1136, 1056, 1023, 954, 907, 839, 762 and 678.
Method of producing aminopolyalkylenephosphonic acid compounds in presence of heterogeneous catalyst / 2384584
Disclosed is a method of producing aminoalkylenephosphonic acid which can be used in water purification, inhibiting scum formation, in detergent additives, sequestering agents, activating additives during oil extraction and as pharmaceutical components. The proposed method of producing aminoalkylenephosphonic acid is realised in the presence of not more than 0.4 wt % hydrohalogenic acid, where all available N-H groups in 50% or more of the amine starting material are converted to the corresponding alkylenephosphonic acid. The proposed method involves reacting (a) phosphorous acid, (b) amine and (c) formaldehyde, where the ratio (a): (b) ranges from 0.05:1 to 2:1, (c):(b) ranges from 0.05:1 to 5:1, and (c):(a) ranges from 5:1 to 0.25:1; where (a) and (c) denote number of moles and (b) number of moles multiplied by the number of N-H groups in the amine, in the presence of a Bronsted acid catalyst which is heterogeneous with respect to the reaction medium, with subsequent extraction of the obtained aminoalkylenephosphonic acid.
 Method of producing mineral salt deposition inhibitor / 2378281
Invention relates to a method of producing mineral salt deposition inhibitors for protecting water circulation systems of enterprises, oilfield equipment and pipelines from mineral deposits, corrosion and biological damage. The method involves reacting ammonia, diethylenetriamine, triethylenetriamine or a technical mixture of polyethylenepolyamines with formaldehyde at temperature ranging from 0 to minus 10°C for two hours, with subsequent reaction with phosphoric acid at 95-96°C, with further neutralisation with sodium hydroxide and addition of methanol and water to the phosphomethylation product, with molar ratio ammonia : formaldehyde : phosphoric acid equal to 1.0 : 2.5-3.0 : 2.5-3.0, diethylenetriamine : formaldehyde : phosphoric acid equal to 1.0 : 5.0 : 5.0, triethylenetriamine : formaldehyde : phosphoric acid equal to 1.0 : 6.0 : 6.0, technical mixture of polyethylenepolyamines : formaldehyde : phosphoric acid equal to 1.0 : 5.0-6.0 : 5.0-6.0.
Treatment of m-(phosphomethyl)glycine / 2369611
Material, containing glyphosate, is diluted or suspended in water in the presence of the base with production of composition, including glyphosate salt in water solution of the base then without preliminary concentration and filtration the produced composition is added into acid and precipitated neutralised glyphosate is separated.
 Polymorphic modification of a ibandronate / 2368617
Invention relates to a new crystalline polymorphic modification of a monohydrate of mon-sodium salt of 3-(N-methyl-N-pentyl)amino-1-hydroxypropane-1,1-diphosphonic acid (ibandronate) of formula 1, used for controlling hypercalcemia.
Method of obtaining alkali metal salts of n-phosphonomethylglycine / 2364601
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.
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.
 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.
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FIELD: chemistry. SUBSTANCE: present invention relates to a method of preparing a zinc complex of disodium or dipotassium salt of hydroxyethylidenediphosphonic acid used as a salting and corrosion inhibitor, in agriculture, medicine and biology. The proposed method is realised using raw products in form of hydroxyethylidenediphosphonic acid, zinc oxide and sodium or potassium hydroxide and is distinguished by that, the raw products are mixed simultaneously while adding zinc oxide and sodium or potassium hydroxide to an aqueous solution of hydroxyethylidenephosponic acid in molar ratio equal to 1:2.2-2.6:1.1-1.3, after which the reaction mass is stirred until complete dissolution, cooled, filtering the residue and an aqueous solution of the zinc complex of disodium or dipotassium salt of hydroxyethylidenediphosphonic acid is obtained. EFFECT: design of an improved method of preparing a zinc complex of disodium or dipotassium salt of hydroxyethylidenediphosphonic acid in form of an aqueous solution. 1 cl, 1 ex
The invention relates to the chemistry of organophosphorus compounds and to methods of producing zinc complexes of alkaline salts hydroxyethylidenediphosphonic acid, used as scale inhibitors and corrosion in agriculture, medicine and biology. The zinc complex of the disodium salt hydroxyethylidenediphosphonic acid (HEDP) described General formula C2H4Na2O7P2Zn. In the industry called eddc-Zn produced product, representing 23-25%aqueous solution of zinc complex eddc (Approvalcan. Heat supply news, 2001, No. 1, p.32), in accordance with TU-2439-001-24210860-97 from 10.07.1997. It is known that in the form of a solid product disodium salt of zinc complex eddc get in a known manner (SU, A.S. No. 790698, C07F 9/38, 1981). This method is carried out in a specific sequence, which, as stated in the description of this method, plays a significant role. In the first stage of this method to aqueous solution eddc add portions of zinc oxide, then the reaction mass was stirred at room temperature for 0.5-1.5 hours, then add aqueous sodium hydroxide solution and the mixture is stirred at room temperature for 2 hours. Source products (eddc, ZnO, NaOH) in this known method, take m is lannom ratio, respectively equal 1,0:0,9-1,0:2,0-2,1. The disodium salt of zinc complex hydroxyethylidenediphosphonic acid (tetrahydrate) are obtained in the form of a crystalline solid product of constant composition with 91,9%output. A method of obtaining 15-23% aqueous solution of the zinc complex of the disodium or Pikalevo salt hydroxyethylidenediphosphonic acid (RU 2305102, C07F 9/38, 2007) reaction of interaction of pre-obtained aqueous solution of zincate sodium or zincate potassium with 20-60% aqueous solution hydroxyethylidenediphosphonic acid is carried out at a temperature of 60-80°C. Original products concat potassium or sodium get in a separate container from 5-20%aqueous solution of potassium hydroxide or sodium and zinc oxide, taken in a molar ratio of 2:1, which is stirred at a temperature of 50-75°C. As can be seen, for the implementation of the known method requires a specific energy consumption, which affects the cost of the final product. In addition, the process in stage 2 reduces the yield of the final product. To create a non-energy-intensive and technologically advanced process developed a new method of obtaining an aqueous solution of the zinc complex of the disodium or Pikalevo salt hydroxyethylidenediphosphonic acid. The proposed method is carried out simultaneously Pach is the use of zinc oxide, hidroxizina sodium or potassium hydroxide with an aqueous solution hydroxyethylidenediphosphonic acid in a molar ratio of 1:2,2-2,6:1-1,3, by stirring the reaction mixture until complete dissolution, cooling, filtration sludge separation and obtain the desired aqueous solution of the zinc complex of the disodium or Pikalevo salt hydroxyethylidenediphosphonic acid. The main difference between the new method from the prototype method is in a different sequence of mixing and consequently the interaction of initial components. A necessary condition for the implementation of the new method is the simultaneous mixing of zinc oxide and hidroxizina sodium aqueous solution hydroxyethylidenediphosphonic acid, which, thanks to ekzotermicheskie response, activates the formation of the target product without additional external heating. This sequence of the process when a certain molar ratio of the reagents makes this method energetically, and therefore it is economically more advantageous than the method-prototype. The difference between the new method from the prototype method is to use a different molar ratio of the starting components. In the new method, the initial products are zinc oxide, sodium hydroxide or potassium and hydroxyethylidenediphosphonic acid take molarnom ratio, respectively equal 1:2,2-2,6:1,1-1,3, that improves the stability hydroxyethylidenediphosphonic acid in time. After cooling, the reaction mass is the deposition of mechanical impurities, which are removed from the solution by the known methods, for example by filtering. Below are examples illustrating the new invention. Example 1 To 1.3 l aqueous solution of HEDP acid containing 226,6 g eddc (100%) under stirring at room temperature simultaneously sprinkled zinc oxide (81,4 g) and sodium hydroxide (88 g) calculation of molar ratio of HEDP: ZnO:NaOH, equal to 1.1:1:2,2. The reaction mass, which due to the exothermic reaction samorazogreva, stirred until complete dissolution of the suspension for 30 minutes, cooled and separated solids from the obtained target product is filtered on a Buechner funnel. Get 1.7 kg of an aqueous solution of the zinc complex of the disodium salt of HEDP acid with a concentration on complex 18,4%. Example 2. To 1.3 l of an aqueous solution of water eddc containing of 267.8 g eddc (100%), with stirring at room temperature simultaneously sprinkled zinc oxide (81,4 g) and potassium hydroxide (104 g) calculation of molar ratios of the reagents eddc: ZnO CON equal to 1.3:1:2,6. Further, the process is carried out analogously to example 1. Get 1.75 kg of an aqueous solution of the zinc complex of potassium is Oli eddc and concentration complex of 17.9%. Thus, experimental studies have shown that the new method has several advantages over the method of the prototype and other counterparts. First, in the new method significantly shortens the duration of the process (up to 45-60 minutes), unlike the prototype, in which the entire process is carried out in a significantly longer time (2 hours or more). Secondly, the process proceeds with the minimum energy cost, since the reaction is exothermic and therefore does not require additional heating for its implementation, in contrast to the prototype method and other analogues. These advantages significantly reduce the cost of the final product and make the process more economical. The resulting aqueous solution is stable during storage and has a high any abscopal effect against deposition of mineral salts and corrosion. The method of obtaining an aqueous solution of the zinc complex of the disodium or Pikalevo salt hydroxyethylidenediphosphonic acid is carried out using as initial products hydroxyethylidenediphosphonic acid, zinc oxide and sodium hydroxide or potassium, characterized in that the starting materials are mixed at the same time, adding zinc oxide and sodium hydroxide or potassium hydroxide to a water solution hydrox ethylidenediphosphonic acid, moreover, the initial products are used in an amount corresponding to the molar ratio of zinc oxide, sodium hydroxide or potassium and hydroxyethylidenediphosphonic acid, equal 1:2,2-2,6:1,1-1,3, then the reaction mass is stirred until complete dissolution, cooled and the precipitate is filtered off from the aqueous solution obtained target product.
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