The method of obtaining butyl acetate |
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IPC classes for russian patent The method of obtaining butyl acetate (RU 2211214):
 The method of producing allylacetate / 2204549
The invention relates to the production of allylacetate high purity based on acetic anhydride
 The method of obtaining second-butyl acetate / 2199521
The invention relates to an improved method for producing sec-butyl acetate is used as solvent for paints and varnishes and as raw material for the production of sec-butyl alcohol
The method of obtaining acetic acid and/or methyl acetate by isomerization and carbonylation / 2181355
The invention relates to the production of acetic acid and/or methyl acetate from a mixture of methanol and methylformate through isomerization and carbonylation
The method of obtaining acetic acid and/or methyl acetate by isomerization of methylformate / 2176635
The invention relates to a technology for production of acetic acid and its derivatives by isomerization of methylformate in the presence of water, aliphatic carboxylic acid WITH1-C10as solvent and catalyst system
 The method of obtaining second-butyl acetate / 2176239
The invention relates to chemical technology, in particular to a method for producing sec-butyl acetate (BWA), used as a solvent for paints and varnishes and for the production of sec-butyl alcohol
 The method of producing acetate and the catalyst for its implementation / 2170724
The invention relates to a method for producing methyl acetate
 Method of regeneration of ethyl acetate / 2166496
The invention relates to the process of extracting the ethyl acetate from the reaction mixtures
 A method of obtaining a carboxylic acid with2- c11or their esters / 2128159
The invention relates to the production of carboxylic acids (C2- C11or the corresponding esters by the interaction of carbon monoxide with at least one reagent selected among alcohols, alkylhalogenide, simple or complex esters, in the presence of a catalytic system comprising at least one rhodium compound and at least one iridium compound or at least one compound containing both metal and at least one halogenated promoter
 The method of obtaining esters and/or mixtures thereof / 2127722
The invention relates to the field of synthesis of esters and/or mixtures thereof
Method of regeneration of ethyl acetate / 2166496
The invention relates to the process of extracting the ethyl acetate from the reaction mixtures
The way to select monoisobutyrate 2,2,4-trimethyl-1,3 - pentanediol from condensation products of aldehyde samalanga / 2082712
The invention relates to the field of chemistry, and more specifically, to method selection monoisobutyrate-2,2,4-trimethyl-1,3-pentanediol from condensation products of samalanga aldehyde in the presence of a catalyst is an aqueous solution of alkali
 Method of extraction of butanol, butyl acetate and water from a mixture of / 2058284
The invention relates to chemical technology, and in particular to methods of separation hardly separated commercial mixtures containing butanol, butyl acetate and impurities, e.g., biological, such as antibiotic products of inactivation, pigments, and can be used in chemical, pharmaceutical, paint and other industries
 The method of producing alkylacrylate (options) / 2161150
The invention relates to an improved process for the preparation of alkylacrylate with high yield and high purity
The method of purification of esters / 2058685
 Drug, possess antiulcer, cardioprotective and anti-shock action / 2211213
The invention relates to medicines, in particular to a mixture of isomers (9)-tetradecanoate
The method of producing allylacetate / 2204549
The invention relates to the production of allylacetate high purity based on acetic anhydride
 The method of obtaining esters of carboxylic acids / 2202536
The invention relates to an improved process for the preparation of esters of carboxylic acids of General formula (I) esterification of the corresponding acids or anhydrides with alcohols in a molar ratio acid:ethanol=1: 0.35 to 2.2 in the presence of hydrocarbons as solvent and aromatic sulfonic acids or acidic sulfate as a catalyst at the boiling temperature of the reaction mixture by distillation of the formed water, followed by washing of the reaction mixture and neutralizing it with an alkaline solution, taken from 5-20 wt
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The invention relates to an improved process for the preparation of butyl acetate by esterification of acetic acid n-butyl alcohol in the presence of an acidic heterogeneous catalyst, separating the resulting reaction water in the form of an azeotrope with azeotropes agent and the selection of the target product, and acetic acid and n-butyl alcohol is fed to the etherification in a molar ratio of 1.00: 1,05, and the process is conducted in two sequential reactors, the first of which is a column type reactor filled with an acidic heterogeneous catalyst, and the second is a reactive distillation reactor, the upper and lower part of which is filled by the nozzle, and the middle part is filled molded cation exchange resin, and in the upper part of the second distillation reactor serves benzene as azeotroping agent. A reliable method can improve the performance of the process and reduce the cost of the target product. 3 C.p. f-crystals, 1 Il.
This invention relates to the field of organic chemistry, namely, the processes of obtaining esters, in particular the production of butyl acetate.
Known methods for producing butyl acetate is actionnow zone in the form of a ternary azeotrope of butanol (a 27.4 wt.%), water (37,3 wt. %), butyl acetate (35,3 wt.%). (N.N. Lebedev "Chemistry and technology of basic organic and petrochemical synthesis, Moscow, Chemistry, 1988, S. 194-207).
A method of obtaining esters of the alcohol and carboxylic acid in the presence of a heterogeneous catalyst (DE 198298809, C 07 C 67/08, 07.01.1999), which is carried out in a distillation column having at the lower part of the reaction zone. Raw material in the column is fed over an area of catalyst, and from the upper rectifying section of the column Argonauts ternary azeotrope containing alcohol, water, ether. The azeotropic mixture is cooled, condensed and separated into organic and aqueous phase. The organic portion contains butyl acetate, butanol and water (solubility), the water part contains n-butyl alcohol (6-8 wt.%), butyl acetate (1 wt.%), which are extracted from water by distillation.
A method of obtaining esters of the alcohol and carboxylic acid, in particular obtaining butyl acetate, in the presence of a homogeneous acid catalyst, for example sulfuric acid, at equimolar ratio of acetic acid and n-butyl alcohol (US 4314947 a, C 07 C 67/08, 09.02.1982). The process is carried out in two reactors, completing the esterification by distillation of the reaction mixture prior is th carboxylic acid and alcohol, as well as the esterification catalyst and formed during the reaction water. The distillation is carried out in the presence or absence of azeotroping agent, which can be used n-butyl acetate, benzene, dichloroethane.
The disadvantages of this method include the stage of a mandatory recycling mixture prior ratifitsirovanie, the triple distillation of the azeotrope, the use of halogen acid catalyst containing corrosive environment, requiring appropriate registration process.
Methods of obtaining esters, in particular butyl acetate, in which the target product from the reaction zone is given in the form of a ternary azeotrope, have several disadvantages are, firstly, the need for a process of esterification with a significant excess of one component (e.g., alcohol), which reduces the efficiency of the process increases the energy consumption for heating of the excess component; and, secondly, the presence of the reaction water content (in the case of obtaining butyl acetate) n-butanol 6-8 wt.%, butyl acetate 1 wt.%, want to extract, resulting in significant additional energy.
A method of obtaining butyl acetate, esterifies in the reaction water in the form of an azeotrope with azeotropes agent and the selection of the target product (SU A3 1240352, 07 WITH 69/14, 1986). In the known method butyl acetate is produced by the esterification of acetic acid with an excess of n-butyl alcohol in the presence of strongly acidic cation exchange resin, followed by distillation of the obtained reaction mixture with allocation as distillate azeotrope with water azeotropes agent toluene, as a side product, displayed below the first plate, the target product in the form of butyl acetate and butanol and as ngacibadyg product withdrawn from distant parts of the column, a mixture of unreacted butanol and acetic acid, is returned to the step of esterification.
However, the known method has the disadvantage consists in the fact that, firstly, the starting mixture for preparing esterification with a significant (0.2 mol) excess alcohol, unreacted alcohol and acid back in the process - this reduces the efficiency of the process and increases the energy consumption.
The use of toluene as azeotroping agent for removal of water has the disadvantage that the azeotrope of toluene and water and the azeotrope of butyl acetate, n-butyl alcohol-water have similar boiling point (84,1 85oAnd 89,4oRespectively), in addition, Tolu is 105,5oC), which also complicates the separation process and requires significant energy consumption for separation of the target product.
The closest in technical essence and the achieved result to the present invention is a method for butyl acetate esterification of acetic acid n-butyl alcohol in the presence of a homogeneous acid catalyst separation resulting from the reaction of water in the form of an azeotrope with azeotropes agent and the selection of the target product (US 4314947, C 07 C 067/08, 1982). In the known method the process is conducted in two units, the first of which represents the reactor, and the second is a reactive distillation column. The process of complete esterification by distillation of the reaction mixture prior tarifitsirovana, which contains in addition to air carbolic acid a number neprevyshenie carboxylic acid and alcohol, as well as the esterification catalyst. When this ester of a specified catalyst contaminated by the products of the hydrolysis catalyst. Useplease from catalyst sulfopropyl together with the reaction water create aggressive corrosion environment, requiring an appropriate design process and leading to sitesee the invention, is to increase the reliability of the method of obtaining butyl acetate, increasing productivity and reducing the cost of the final product.
The technical result of the invention is to improve the performance of the process, increasing the purity of the finished product and reduce energy consumption.
The specified task with the achievement of the technical result is solved in a method of producing butyl acetate esterification of acetic acid n-butyl alcohol in the presence of an acidic heterogeneous catalyst, separating the resulting reaction water in the form of an azeotrope with azeotropes agent and the selection of the target product the fact that acetic acid and n-butyl alcohol is fed to the etherification in a molar ratio of 1.00:1,05, and the process is conducted in two sequential reactors, the first of which is a column type reactor filled with an acidic heterogeneous catalyst, and the second is a reactive distillation reactor, the upper and lower part of which is filled by the nozzle, and the middle part is filled molded cation exchange resin, and in the upper part of the second distillation reactor serves benzene as azeotroping agent.
In addition, the use of the nozzle of Sulzer.
In the area of acidic heterogeneous catalyst is preferably maintain the temperature 90110oAnd in the area of the molded cation exchanger 9095oC.
It is also advisable benzene to file in the upper rectifying part of the reactive distillation reactor in an amount necessary for the formation of the azeotropic mixture of benzene-water.
The advantage of using benzene as azeotroping agent with water in the environment butyl acetate, n-butyl alcohol-water-acetic acid is the fact that benzene with any of these substances, except water, does not form azeotropic mixture, and the resulting azeotropic mixture of benzene-water has a boiling point significantly different from the boiling point of the remaining components of the mixture, which increases the reliability of the process.
In Fig. 1 shows a diagram of the setup for the esterification of acetic acid n-butyl alcohol, 1 - flow reactor; 2 - reaction-nitrifikatsionnuyu reactor; 3 - head azeotropic distillation (with capacitor and fasoracetam); 4 - condenser-refrigerator; 5 - receiver butyl acetate raw; 6 - a mixture of alcohol and acetic acid.
Device for producing butyl acetate consists of two p is Roccia 0,3151.25 mm 60 g of dry volume bulked up to 195 cm3), and reactive distillation reactor 2 with a diameter of 45 mm, the upper and the lower part of which is filled with a nozzle of Sulzer and function of the distillation column (efficiency), 12 m.m. each), and the middle part of the reaction zone is filled molded cation exchange resin (tablet size 5 mm) in an amount of 35 g of 100 cm3.
Raw materials - acetic acid and n-butyl alcohol in a molar ratio of 1: 1,05 served in the upper part of the once-through reactor 1, which gives the reaction mixture with the equilibrium degree of conversion. The products of direct-flow reactor served in the middle part of the reactive distillation reactor 2 over an area molded cation, and in the upper rectifying part of the reactor from the head 3 irrigation serves benzene in an amount necessary for the formation of the azeotropic mixture of benzene-water and output water from the reaction mixture.
Azeotropic mixture of benzene-water is diverted from the upper rectifying part. After condensation, cooling and phase separation of the mixture in patristical benzene is fed to irrigation, water is removed from the system.
The target product of butyl acetate raw divert from p> In once-through reactor 1 column type, filled with strongly acidic cation exchange resin KU-2-8 (fraction 0,3151.25 mm 60 g of dry volume bulked up to 195 cm3) serves 276 g/h heated mixture of n-butyl alcohol and acetic acid in a molar ratio of 1.05:1.0, the process of esterification is carried out at a temperature of 90110oC. the reaction Products from the once-through reactor served in the reactive distillation reactor 2, the upper and the lower part of which is filled with a nozzle of Sulzer, and the middle part is filled with cation exchange resin molded over the area molded cation, in the zone of the catalyst KU-2-8 support temperature 90110oWith, in the area of the molded cation exchanger 9095oWith, cubed 125130oC.
The reaction water is distilled off from the top of the distillation column at a temperature of 6971oWith as azeotropic mixture with benzene, which serves in the number of 403 g/h
Azeotropic mixture in the separator splits into water and the benzene phase. Water in the amount of 36 g/h is displayed, the benzene is returned to irrigate the upper rectifying part.
Butyl acetate, and the temperature is 125128oC.
The resulting butyl acetate raw has a composition, wt.%: Butyl acetate - 98,0 n-butyl alcohol - 1,7 Neizvestnye impurity - 0,3Eat butyl acetate with 1 kg of catalyst is 2.4 kg/h, in the process there is no recycling of raw materials; in distilled water, the reaction products are not available, the content of benzene in water is 0.05 wt.%. Industrial applicability The present invention can be implemented using known means and is most effectively used in the production of esters, in particular butyl acetate.
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