Method of producing mineral salt deposition inhibitor |
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IPC classes for russian patent Method of producing mineral salt deposition inhibitor (RU 2378281):
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.
 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.
 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: oil and gas industry. SUBSTANCE: 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. EFFECT: design of a new, effective, non-waste and cheap method of producing salting inhibitors. 3 cl, 8 ex, 1 tbl
The invention relates to the chemistry of phosphorus compounds used as inhibitors of deposits of mineral salts to protect water recycling systems, oil field equipment and pipelines from the mineral deposits, corrosion and biological lesions, which are the major problems and lead to frequent breakdowns and expensive equipment, the production of defective products, increase energy consumption, etc. Known methods for producing solid disodium salt of nitrilotriethanol acid (NTF) with prior NTF-acid, for example, the interaction of ammonia, formaldehyde and compounds of trivalent phosphorus [RF Patent №2131433] and trinitarios salt nitrilotriethanol acid [RF Patent №2056428]. The disadvantages of the known methods of obtaining inhibitors of deposits of mineral salts are the unavailability of raw materials, namely, compounds of trivalent phosphorus. Closest to the claimed method according to technical essence and the achieved results is a method for inhibiting deposits of mineral salts by the interaction of derivatives of ammonia, including ammonium chloride or waste production polyethylenepolyamines, with formaldehyde and phosphorous acid as such or a product of hydrolysis of trichloric the th of phosphorus in the environment of diluted hydrochloric acid at elevated temperature, followed by neutralization of the resulting solution hydroxide Na to pH 6.5±1.0 in. The process is conducted at a molar ratio of the initial reagents - ammonia: formaldehyde: phosphoric acid 1,0:2,35-2,65:2,2-2,4 [RF Patent №2133751]. The disadvantage of this method is to conduct the process at a high temperature and unavailability of raw materials, namely phosphorous acid, insufficient efficiency of inhibition. The objective of the invention is the development of a waste-free method of obtaining inhibitors of deposits of mineral salts, improve the protection of water recycling systems, oil field equipment and pipelines from the mineral deposits, the expansion of raw materials, the simplicity of instrumentation. The technical result in the use of the invention is expressed in non-waste technology for deposition inhibitors of mineral salts, the improvement inhibiting properties and possible use of available raw materials. The above result of receiving inhibitors of deposits of mineral salts, working in saline environments is achieved by the fact that ammonia water, private polyamine, in particular Diethylenetriamine (DETA), Triethylenetetramine (THETA) or a technical mixture of polyethylenepolyamines (PET) molecular weight: 108 (light fraction of probes), or a technical mixture of probes with molecular mass: 148,64 (the average fraction of probes), subject entries batch is Yu with formaldehyde and phosphorous acid Paladino. The chemistry of the process describes a General scheme:
This results in the Tris(methylphosphate)Amin. As NH3use ammonia: ammonia water, private polyamine, in particular Diethylenetriamine, Triethylenetetramine and technical mixture of polyethylenepolyamines. In the first stage at a temperature 0 ÷ -10°C to aqueous solution of ammonia, individual amines (DETA or THETA) or technical mixtures of probes slowly pin aqueous solution of formaldehyde (formalin) and stirred for 2 hours. Then the temperature in the reactor was raised to 95-96°C and at the same temperature dosed phosphoric acid. Stirring is continued at this temperature for 2 hours. Carry out neutralization with caustic soda to a pH of 6-7. The process is conducted at a molar ratio of the initial reagents: 1) ammonia: formaldehyde: phosphoric acid 1,0:2,5-3,0:2,5-3,0; 2) DETA: formaldehyde: phosphoric acid 1,0:5,0:5,0; 3) THETA: formaldehyde: phosphoric acid 1,0:6,0:6,0; 4) technical mixture of probes: formaldehyde: phosphoric acid 1,0:5,0-6,0:5,0-6,0. Then the reaction mixture is cooled, mixed with the solvent of methyl alcohol and water. The peculiarity lies in the fact that the raw material used phosphoric acid, private polyamine, in particular Diethylenetriamine (D IS TA), triethylenediamine (THETA) and the technical mixture of probes, and the stage of the methylation is carried out at low temperature. The advantages of the proposed method compared to the base object are: - high efficiency of the inhibitor; low temperature curing inhibitor; - availability of raw materials used in the synthesis of the scale inhibitor; - no waste in the proposed process of obtaining inhibitor; - synthesis in soft without technological difficulties; the simplicity of instrumentation. The method is illustrated by the following examples. Example 1. In the reactor (three-neck flask)equipped with a mechanical stirrer, reflux condenser, thermometer, jacket cooling (heating) load 34 g (0.5 mole) of ammonia in the form of a 25%aqueous solution and slowly added dropwise at 0°With 101,35 g (1.25 mol) of formalin. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise of 122.5 g (1.25 mol) of phosphoric acid. Stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7. Add 158,34 g of water and 204,5 g of methanol, stirred at room temperature for 0.5 to 1 hour. Determine the effectiveness of the inhibitor deposits m the mineral salts. The results are shown in the table. Example 2. In the conditions of example 1 was charged to the reactor 34 g (0.5 mole) of an aqueous solution of ammonia and slowly added dropwise at a temperature of -5°C to 121.6 g (1.5 mol) of formalin. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise 147 g (1.5 mol) of phosphoric acid. Stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7, add 232,7 g of water, to 240.5 g of methyl alcohol and stirred at room temperature for 0.5-1 hour. The efficiency shown in the table. Example 3. In the conditions of example 1 was charged to the reactor 25,75 g (0.25 mol) of DETA and slowly added dropwise at 0°With 101,35 g (1.25 mol) of formalin. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise of 122.5 g (1.25 mol) of phosphoric acid. After filling, stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7, add 227,57 g of water and 256,9 g of methyl alcohol and stirred at room temperature for 0.5-1 hour, after which determine efficiency. The results are shown in the table. Example 4. In the conditions of example 1 was charged to the reactor is of 36.5 g (0.25 mole) of THETA and slowly added dropwise at a temperature of -10°C to 121.6 g (1.5 mol) of formalin. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise 147 g (1.5 mol) of phosphoric acid. After filling, stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7, add 295,8 g of water and 323,59 g of methyl alcohol and stirred at room temperature for 0.5-1 hour, after which determine efficiency. The results are shown in the table. Example 5. In the conditions of example 1 was charged to the reactor 27 g (0.25 mol) of a technical mixture of polyethylenepolyamines (PET) with a molecular mass of 108 (light fraction of probes) and slowly added dropwise at 0°With 101,35 g (1.25 mol) of formalin. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise of 122.5 g (1.25 mol) of phosphoric acid. After filling, stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7, add water and methyl alcohol. The results are shown in the table. Example 6. In the conditions of example 1 was charged to the reactor 27 g (0.25 mol) of a technical mixture of polyethylenepolyamines (PET) with a molecular mass of 108 (light fraction of probes) and slowly pinned at a temperature of -10°C 101,35 g (1.25 mol) is armaline. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise of 122.5 g (1.25 mol) of phosphoric acid. After filling, stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7, add methyl alcohol and water, and then determine the effectiveness of the inhibitor deposits of mineral salts. The results are shown in the table. Example 7. In the conditions of example 1 was charged to the reactor 37,16 g (0.25 mol) of a technical mixture of polyethylenepolyamines (PET) with a molecular mass of 148,64 (the average fraction of probes) and slowly added dropwise at a temperature of 0°C to 121.6 g (1.5 mol) of formalin. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise 147 g (1.5 mol) of phosphoric acid. After filling, stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7, add methyl alcohol and water, and then determine effectiveness. The results are shown in the table. Example 8. In the conditions of example 1 was charged to the reactor 37,16 g (0.25 mol) of a technical mixture of polyethylenepolyamines (PET) with a molecular mass of 148,64 (the average fraction of probes) and slowly added dropwise at a temperature of -10°C 1216 g (1.5 mol) of formalin. After dosing at the same temperature stirring is continued for 2 hours. Then in the reactor to raise the temperature up to 95-96°C and added dropwise 147 g (1.5 mol) of phosphoric acid. After filling, stirring is continued at a temperature of 95-96°C for 2 hours. Carry out neutralization with sodium hydroxide to a pH of 6-7, add methyl alcohol and water, and then determine effectiveness. The results are shown in the table. 33% active basis (AO), 35% methyl alcohol, 32% water
1. The method of obtaining inhibitor deposits of mineral salts by postmaterialism nitrogen compounds, characterized in that as the nitrogen compounds used ammonia or Diethylenetriamine, or Triethylenetetramine, or a technical mixture of polyethylenepolyamines, which is subjected to interaction with formaldehyde at a temperature 0 ÷ -10°C for two hours, followed by interaction with phosphoric acid at a temperature of 95-96°C, with subsequent neutralization with sodium hydroxide and relax the tion to the product postmetallocene methyl alcohol and water, moreover, the process of postmetallocene carried out at a molar ratio of 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, Triethylenetetramine: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. 2. The method according to claim 1, characterized in that as a technical mixture of polyethylenepolyamines use light or medium fractions with a molecular mass of 108 and 148,64 respectively. 3. The method according to claim 1, characterized in that the product postmetallocene, methyl alcohol and water take in a weight ratio, wt.%: 33-39:31-35:30-32.
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