The method of producing salt water corrosion inhibitor
(57) Abstract:The invention relates to methods for inhibitor salt corrosion. The proposed method lies in the interaction of chloroalkanes received by hydrochloridebuy fraction of higher fatty alcohols, Ethylenediamine in water when heated, and a hydrocarbon chain chloroalkanes contains 12 to 14 carbon atoms, and the process is conducted at a temperature of 150-160oAnd pressure 0,55-0,65 MPa. The amount of water is 5-15% by weight of the starting materials, preferably 10%. The resulting inhibitor has a high protective effect and bactericidal activity against corrosive sulfate-reducing bacteria. 1 C.p. f-crystals, 3 tables. The invention relates to methods for inhibitor salt corrosion from chloroalkanes with alkyl radical C12-C14and Ethylenediamine.A method of obtaining alkyl derivatives of diamines having the formula:
< / BR>where R1, R2, R3, R4are the same or different alkyl radicals containing from 8 to 30 carbon atoms or at least one of them is a hydrogen atom, and p is 2 - 12 (U.S. Pat.The UK 2048861, opetator hydrogenation, for example, Nickel, and solvent, such as methanol, by heating under hydrogen pressure.Also known is a method of obtaining N-alkylamidoamines reaction of ethylene diamine with an alkyl halide C3-C6when a molar ratio of (1 - 20) : 1 and a temperature of from -10 to 120oC in the presence of 0-50% water by weight of the original substances (Germany, application 2929841, publ.18.12.80). The resulting reaction mixture is neutralized inorganic alkaline agent. The aqueous layer was separated from the neutralized organic layer. The organic layer type hydrocarbon solvent and azeotropic distillation to remove water and Ethylenediamine. To allocate N-alkylamidoamines pure hydrocarbon is distilled off.Obtained in this method, the products contain one alkyl radical with small (C3) or relatively small (C6) molecular weight, combined with a low molecular weight group of ethylene diamine. These products are corrosion inhibitors. In addition, in the method (the Federal Republic of Germany, application 2929841) used a large number of operations when selecting a product, which complicates the technology of its production and increases the cost of the product. The solvent makes the process more fire and vzryvoopasen mixture of aminopropanol, containing 1 to 6 amino groups, as a corrosion inhibitor (Patent RF 2074170, publ.27.02.97). A mixture of aminopropanol obtained by aminating the product of chlorination of liquid chloride liquid paraffins C10-C26with their boiling temperature 220-345oC carbamide deparaffinization. Amination of chlorinated paraffin wax spend Ethylenediamine, Triethylenetetramine and O-[N,N-bis-(2-amino-ethyl)-aminomethyl]-phenol in the wall under atmospheric pressure at a temperature of 120-160oC in the presence of a catalyst - copper filings with the subsequent processing of the reaction products in an aqueous solution of sodium hydroxide, separating the aqueous layer from the organic and Stripping of the organic layer from Ethylenediamine and traces of moisture.However, the effectiveness of a mixture of aminopropanol as corrosion inhibitor obtained, as indicated in the patent of the Russian Federation 2074170 method is not high enough: the protective effect of the compositions at concentrations in inhibiting solution 250 mg/l for 6 hours 86,3-94,5%. In addition, this method is characterized by a large number of operations used to highlight key products.Object of the present invention to provide a highly effective corrosion inhibitor.The advantage of the proposed method is that as a result of heating at a temperature of 150-160oC chloroalkanes with alkyl radical C12-C14and Ethylenediamine is formed a mixture of alkyl substituted Ethylenediamine containing a large number (more than 90 wt.%) di-, tri - and tetraalkylammonium with a high molecular weight, having a good protective effect in corrosion of metallic materials.The solubility of mixtures of high-molecular alkylamino in water and water in the mixture is practically zero, and the solubility of ethylene diamine and salts of Ethylenediamine in water is high, which significantly simplify the process at the stage of selection of the target product.The invention is illustrated by the following examples.Example 1-6.In a metal reactor, the heated coolant, download chloralkali fraction C12quantities listed in table. 1. The contents of the reactor are heated at a temperature of 140-160oC for 13-15 hours. The reaction course is monitored by the amount of released hydrochloric salt of ethylene diamine (Seda), which octarepeat of 0.1 n alkali solution. Upon completion of the reaction the mixture is heated to ~80oC, poured into a separating volanco, in which are formed two layers: the upper organic layer containing the target product, unreacted chloralkali and impurities, and the lower layer of water containing the Ethylenediamine salt and Ethylenediamine. The bottom layer is separated and sent to the regeneration of Ethylenediamine from its salts by reaction with concentrated alkali solution.The organic layer is poured from a separating funnel at a temperature above the 50oC and analysed. The chromatographic analysis is performed on the non-polar phase.For rapid analysis of the finished product using the titration of a sample of 0.1 N. hydrochloric acid. The specific parameters of the process and its results are presented in table.1. The process is outside of the settings specified in the claims, reduces the yield of the target product.The finished product is a pasta sicredi product composition, obtained under optimum conditions (op.4, PL. 1) and with the highest technical indicators, presented in table 2.Anticorrosive action of a mixture of alkylamidoamines determined in the laboratory gravimetric method and the use of steel (steel grade 08 KP) plates 50 x 10 x 0.5 mm on the model of the water, imitating the produced water composition, g/l: Na+- 3,500; Ca2+- 0,056; Mg+2- 0,074; Cl-- 4,960; HCO3-- 1,461; CO32-- 0,024 and total mineralization of 10.1 g/l Concentration of product in inhibiting solution was and is 25.50 100 mg/l, the corrosion Rate of the control sample in eingeborenen model produced water for 6 hours was equal 0,972 g/m2including the results of the tests are presented in table 3.Thus, the technical result of the invention is superior to the nearest equivalent to ten times (at a concentration equal to 25 mg/l proposed inhibitor, a protective effect is 93,5%, and a similar effect to 87.1% at a concentration of 250 mg/l).In addition, it was found that the resulting mixture of alkyl substituted Ethylenediamine has bactericidal activity against corrosive SRB "ptx2">High corrosion resistance and antibacterial activity of the product is recommended for use in oil production. 1. The method of producing salt water corrosion inhibitor interaction chloroalkanes with Ethylenediamine in aqueous medium at a temperature of 150 - 160oC, wherein the carbon chain of chloroalkanes contains 12 to 14 carbon atoms, and the process is conducted at a pressure 0,55 - 0,65 MPa.2. The method according to p. 1, characterized in that the amount of water is 5 to 15% by weight of the original substances, preferably 10%.
FIELD: organic chemistry, chemical technology, pharmacy.
SUBSTANCE: invention relates to derivatives of allylamines, namely, to a method for preparing terbinafine or its hydrochloride. Method involves interaction of N-methyl-naphth-1-yl-methylamine taken in excess with 1-halogen-6,6-dimethylheptene-2-ene-4-ine in water or inorganic base an aqueous solution followed by, if necessary, treatment of prepared product with hydrochloric acid. As a rule, as the parent reagent both 1-bromo-6,6-dimethylhept-2-ene-4-ine and 1-chloro-6,6-dimethylhept-2-ene-4-ine is used. Usually 5-50% mole excess of N-methyl-naphth-1-yl-methylamine is used in case using inorganic base. Method provides enhancing yield of the end compound, to simplify the process and to expand the raw base by using the more low-priced 1-chloro-6,6-dimethylhept-2-ene-4-ine as an alkylating agent.
EFFECT: improved preparing method.
3 cl, 3 ex
FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to the improved method for synthesis of N,N,N',N'-tetramethyl-1,2- and -1,3-propylenediamines. Method involves interaction of 1,2-dichloropropane or 1,3-dichloropropane with 36-38% an aqueous solution of dimethylamine heated preliminary to temperature 105-110°C wherein 1,2-dichloropropane or 1,3-dichloropropane is added to dimethylamine solution. Synthesis is carried out at temperature 120-125°C and under pressure 0.5-1.1 MPa in the mole ratio of reagents dichloropropane : dimethylamine = 1:(2.1-2.9). Preferably, synthesis is carried out at intensive stirring with rotation number of a mixer 600-2800 rev/min. Method provides enhancing yield and purity of synthesized product and intensifying the process.
EFFECT: improved method of synthesis.
2 cl, 5 ex
SUBSTANCE: invention relates to improved method of obtaining N,N,N'N'-tetramethylentylenediamine, which can be applied for obtaining hardeners of epoxy resins and polyurethanes, corrosion inhibitors, lubricants, textile-auxiliary substances, emulsifiers, disinfecting and bactericidal preparations. Method of invention lies in the following: 1,2-dichlorethane is dosed with mixing to heated up to 95-104°C 30-36% water dimethylamine solution, reaction mixture is stood at temperature 111-119°C and pressure 0.4-0.9 MPa during 1-2 hours with molar ratio DCE:DMA=1:3÷3.5. It is desirable to carry out synthesis with number of mixing device revolutions 800-3000 rev/min.
EFFECT: target products with increased output and of high quality, and reduction of process duration.
2 cl, 5 ex
SUBSTANCE: invention relates to a novel method of producing hydrochlorides of amine-derivatives of adamantane of general formula:
where R=H, CH3; n=0, 1. According to the disclosed method, biologically active compounds such as, for example, hydrochlorides of 1-aminoadamantane (R=H, n=0) (amantadine) and 1-amino-3,5-dimethyl-adamantane (R=CH3, n=0) (memantine) are obtained, which are used in the chemical and pharmaceutical industry to prepare medicinal agents for treating Parkinson's disease, Alzheimer's diseases, neurodegenerative diseases, glaucoma etc. The method involves reaction of adamantane carboxylic acid with thionyl chloride at its boiling point for 1.5 hours in molar ratio 1:1.1 respectively, to form an acyl chloride of adamantane carboxylic acid, which reacts with sodium azide in anhydrous toluene at its boiling point in molar ratio 1:1:15-20 respectively for 1.5-2 hours, followed by addition of concentrated hydrochloric acid and holding the reaction mass for 1 hour and extracting the end product.
EFFECT: method is more technologically effective and ecologically clean and enables to obtain a large number of homologues of hydrochlorides of amine-derivatives of adamantane with quantitative output of 92-95%.
SUBSTANCE: invention relates to an improved method for ammonolysis of chlorohydrocarbons by reacting chlorohydrocarbons and ammonia to obtain a solution of aminochlorohydrates and ammonium chloride, neutralising that solution and separating amines. Before the neutralisation step, the solution of aminochlorohydrates and ammonium chloride undergoes at least four-step cooling: at the first step to temperature 20-25°C and holding at that temperature for about 30 minutes, followed by slow cooling at a rate of 4-5°C/h to temperature 10°C at the second step and holding at that temperature for 2 hours while stirring, further cooling at a rate of 10°C/h to temperature minus 10°C at the third step and holding for 1 hour and cooling at the fourth step to temperature minus 25°C and holding for 1 hour. Further, the solution of aminochlorohydrates is separated from the crystallised ammonium chloride by filtration and taken to the neutralisation step, and ammonium chloride is purified. At the purification step, ammonium chloride is washed with hydrochloric acid with weight ratio of HCl of 20-36% and weight ratio of ammonium chloride to acid equal to 1:2, followed by holding the mixture until formation of layers, separating ammonium chloride from hydrochloric acid and drying until all moisture is removed.
EFFECT: method reduces the amount of sodium chloride formed at the step for neutralising products of ammonolysis of chlorohydrocarbons, reduces the amount of waste water, increases energy efficiency of the process, and also increases output of amines and enables to obtain an additional commercial product in form of ammonium chloride.
6 cl, 5 ex
SUBSTANCE: reaction mixture of aqueous solutions of ammonia and ethylenediamine is heated to 90-104°C while stirring; under said conditions, dichloroethane is added with molar ratio dichloroethane:ammonia:ethylenediamine=1:1.5-2.5:0.3-0.7 for 1-2 hours; while stirring, the reaction mixture is then held at 110-130°C and pressure 0.6-2.5 MPa for 1.5-2 hours.
EFFECT: method increases selectivity of the process and enables to obtain a product with high output.
3 cl, 8 ex
SUBSTANCE: obtained as a result of the interaction an aminohalogenhydrate solution is processed with an alkali with the further evaporation and rectification. Sewage water, which represents a light fraction, formed on an upper plate of a rectification column and contains about 2% of ammonia and about 1% of ethylenediamine, is subjected to electrochemical processing in a three-chambered membrane electrolyser with ion-exchange membranes with the current density 130-500 A/m2 with the supply of sewage water into an anode chamber, the alkali into a cathode chamber, and water into a middle chamber. A concentrated solution of ethylenediamine with ammonia is separated from the middle chamber and directed to obtaining a water ammonia solution, used in the production of amines. The method makes it possible to reduce the volume of sewage waters, eliminate the loss of amines and ammonia with sewage waters. The amines and ammonia are separated almost completely. Sewage waters can be discharged into a plant sewage system without dilution.
EFFECT: method improvement.
1 dwg, 3 tbl, 3 ex
SUBSTANCE: invention relates to novel trihydrochlorides of (R)- and (S)-isomers of 1,8-diamino-3-methyl-4-azaoctane (3-methylspermidine), corresponding to structural formulae given below and to a method for production thereof. Said compounds can be used in vitro and in vivo to investigate individual cell functions of easily interconvertible and partially interchangeable spermine and spermidine, which are vital for tumour cells and pathogenic trypanosomatids. The (R)-isomer of 3-methylspermidine trihydrochloride is the first metabolically stable functionally active spermidine mimetic.
. A method of producing said isomers includes alkylating salts of (R)- and (S)-isomers of N1-protected 1,3-diaminobutane sulphamide with N-protected 1-amino-4-butylhalides, followed by successive removal of protective groups and treatment of the obtained residue with hydrochloric acid solution. The alkylating agent used can be N-(phthaloyl)-1-amino-4-butylhalides in aprotic polar solvents or N-(4-iodobutyl)phthalimide in dimethyl formamide in the presence of calcium carbonate. Removal of the phthalyl protection is normally carried out with hydrazine hydrate in alcohol. Removal of benzyloxycarbonyl groups is normally carried out by catalytic hydrogenation over Pd-black at atmospheric pressure in a mixture of methanol and acetic acid.
EFFECT: converting the obtained triacetates of R)- and (S)-isomers of 1,8-diamino-3-methyl-4-azaoctane into tetrahydrochlorides is carried out with aqueous hydrochloric acid solution.
7 cl, 5 dwg, 5 ex
SUBSTANCE: invention relates to an improved method of producing aliphatic di- and polyamines, used in production of corrosion inhibitors, succinimide additives, amine curing agents, ion-exchange resins etc. Method is realised by reacting dichloroethane or 1,2-and 1,3-dichloropropanes and 25–45 % solution of ammonia in molar ratio of reactants of 1:2.2–4 at high temperature and pressure, followed by neutralising obtained reaction mixture. Reaction of dichloroethane or 1,2 and 1,3-dichloropropanes with ammonia is carried out in presence of a stabiliser, in form of 2,6-ditertbutyl-4-methylphenol (ionole) or 2,6-ditretbutylphenol in amount of 0.1 % of weight 1,5-dichloroethane or 1,2 and 1,3-dichloropropanes, and process is first carried out at temperature of 106–110 °C and pressure 0.4–0.8 MPa for 1–1.5 h, reaction mixture is held at 110–140 °C and pressure of 0.6–1.8 MPa for 1-2 hours with intense mixing. Mixing of reaction mixture is primarily performed with rotation frequency 600–3,000 rpm.
EFFECT: method increases output of ethylene and propylene polyamines to 80,6–96,2% due to reduced formation of by-products - ammonium chloride, vinyl chloride, monochloropropenes.
1 cl, 1 tbl, 10 ex
FIELD: organic chemistry, chemical technology.
SUBSTANCE: invention relates to the improved method for preparing aliphatic amines by addition reaction of ammonia to (C2-C8)-alkenes, for example, to isobutylene in gaseous phase and reaction is catalyzed by heterogeneous, preferably zeolite catalyst. Process is carried out in system comprising two sections - separating and reaction that are interrelated and interdependent and one cooling zone working under the same pressure from 2 to 8 MPa. Liquid mixture of ammonia and alkene is fed to upper part of separating section fitted with dephlegmator and then mixture is fed to reaction section containing catalyst, for example, zeolite catalyst of type ZSM-5 wherein alkene reacts with ammonia partially and forms amine. Temperature in reaction section is maintained usually from 220oC to 320oC and the molar ratio of ammonia to alkene at inlet to reaction section is from 1.5 to 20 usually. Then reaction mixture removing reaction section is cooled in cooling zone to temperature about the condensation point by heat-exchange with mixture that is recovered for repeated utilization from separating section to reaction section. Cooled reaction mixture is recovered to separating section fitted with built in packing for intensification of mutual contact of countercurrent of liquid and gaseous phases wherein the amine concentrate is separated from reaction mixture and removed from heated vat of separating section. Indicated concentrate is purified additionally and unreacted mixture of alkenes and ammonia in common with fresh parent compounds is recovered for repeated processing in gaseous form from condenser of this section to reaction section. Method provides reducing energy consumptions due to reducing heat consumptions and pressure.
EFFECT: improved preparing method.
12 cl, 1 dwg, 2 ex
FIELD: organic chemistry.
SUBSTANCE: target products is produced by ethylene diamine transamination. Reaction is carried out at 135-180°C at pressure of 5-40 MPa in presence of hydrogen and catalyst particles containing 26-65 wt.% of metallic nickel on porous carrier.
EFFECT: high ethylene diamine conversion ratio and high selectivity in relate to target acyclic polyethylene polyamines under advantageous reaction conditions.
10 cl, 2 tbl, 1 ex
SUBSTANCE: proposed invention pertains to organic chemistry, more specifically to the method of producing N,N-dimethyl-3-phenyl-2-propyne-1-amine. The method involves reacting phenylacetylene with excess bisamine in the presence of a vanadyl acetylacetonate catalyst (VO(acac)2) in an argon atmosphere at 85°C temperature and atmospheric pressure for a period of 4-8 hours. N,N-dimethyl-3-phenyl-2-propyne-1-amine output is 84-98%.
EFFECT: invention can be used in thin organic synthesis, particularly for making not easily accessible polycyclic compounds, as well as in synthesis of biologically active substances.
1 tbl, 1 ex
SUBSTANCE: invention relates to an improved method of producing N,N,N,N-tetramethylalkadiynediamines, which can be used in fine organic synthesis, particularly for producing not easily accessible polycyclic compounds, as well as in synthesis of biologically active substances. Desired compounds are obtained from reacting diacetylene alkanes with excess N,N,N,N-tetramethylmethane diamine in the presence of a vanadyl acetylacetonate (VO(acac)2) catalyst, in molar ratio diacetylene alkane: N,N,N,N-tetramethylmethane diamine: VO(acac)2 = 10:(25-35):(0.2-0.4) in an argon atmosphere at temperature ranging from 70 to 100°C, mostly at 80°C, and atmospheric pressure for 4 to 8 hours.
EFFECT: method considerably simplifies synthesis schematic due to use of accessible initial reagents and significantly increases output of desired products, and allows for obtaining new and known compounds.
1 cl, 3 dwg, 1 tbl, 1 ex
SUBSTANCE: invention relates to an improved method of producing N1,N1,N4,N4-tetramethyl-2-butyne-1,4-diamine, which is used in synthesis of polycyclic compounds, as well as in synthesis of biologically active substances. The method involves reaction of N,N,N,N-tetramethylmethane-diamine with excess gaseous acetylene in the presence of a VO(acac)2 catalyst, taken in molar ratio of N,N,N,N-tetramethylmethane-diamine: (VO(acac)2) = 10 : (0.3-0.5), preferably 10:0.4, at temperature 65-75°C and atmospheric pressure for 1-3 hours.
EFFECT: method increases output of the desired product.
1 cl, 3 dwg, 1 tbl, 1 ex
SUBSTANCE: method involves reaction of bisamine with 3-fold excess acetylene in the presence of a vanadyl acetylacetonate (VO(acac)2) catalyst in an argon atmosphere at temperature 70°C and atmospheric pressure for 3 hours, followed by addition of diisobutylaluminium hydride and stirring the reaction mixture for 4-6 hours at room temperature. The method enables to obtain N1,N1,N4,N4-tetramethyl-2-butene-1,4-diamine from available reagents with quantitative output of (82-97%).
EFFECT: high output of end product.
1 tbl, 3 dwg, 1 ex
SUBSTANCE: present invention relates to versions of a method of purifying terbinafine from nonmetallic impurities, primarily a substance A of formula
, as well as to use of said methods to obtain purified terbinafine. One of the versions of the method involves molecular distillation of crude terbinafine in form of a free base and extraction the obtained purified terbinafine in form of a free base or acid-addition salt (method A). In another version (method B), crude terbinafine in form a free base undergoes molecular distillation combined with formation of a salt of the obtained product with simultaneous deposition of a purified trans-isomer, and the obtained highly pure terbinafine is extracted in form of a free base or acid addition salt.
EFFECT: method enables to obtain terbinafine containing less than approximately 5 ppm of substance A.
13 cl, 2 dwg, 6 ex