The method of purifying ethyl alcohol
(57) Abstract:Use: in the production of aliphatic alcohols in particular in the method of purification of ethanol. The inventive product is ethanol, BF C2H6O the content of carbonyl impurities 1 to 4.5 mg/l reaction Conditions: purification of ethanol are processing its hydrocyclon alkali metal and sodium borohydride, taken in an amount of 0.01 to 0.1 and 0.005 to 0.3 wt. accordingly, 1 Il. table 1. The invention relates to a method of purification of ethanol from carbonyl impurities by treating it with a chemical reagent, rectification and can be used in the production of ethyl alcohol and in the processes of organic synthesis using ethyl alcohol.Currently, the domestic industry of ethyl alcohol is produced by fermentation of food raw materials, hydrolysis of plant materials, direct hydration of ethylene in the presence of acid catalysts. In all cases, at the stage of synthesis of the target product are formed such side products, such as aldehydes (carbonyl compounds), higher alcohols, with the most contaminated aqueous-alcoholic raw is formed by synthetic ethyl spyrestudios technological scheme and this, along with the purified ethyl alcohol are formed contaminated with aldehydes and other impurities alcoholic solutions, which result in losses of the target product, and the selection of the target product from them effectively can be chemical or adsorption methods. The most difficult is the process of separating the purified ethyl alcohol from water and raw alcohol formed during the direct hydration of ethylene, which, along with the target product contains a number of carbonyl compounds with a wide limit of the boiling points acetaldehyde, acetone, propionic aldehyde, methyl ethyl ketone, CROTONALDEHYDE and other Synthetic ethyl alcohol, manufactured now on THE 38.402-62-117-90 and containing in their structure a wide range of carbonyl compounds, is widely used in the processes of organic synthesis, thus there is often the need for cleaning of the product from the carbonyl impurities.The most known method of purification of ethanol from organic impurities, including aldehydes, ketones, is the method of cleaning, comprising the stage of dilution of the concentrated ethyl alcohol and water passing through the layer of activated carbon  Usually this method is used for the purification of ethanol from the concentration of the cleaning heavily soiled product due to the low sorption capacity of coal and selective absorption of impurities, this method is inefficient, includes stage dilute the alcohol with water, and subsequent concentration of alcohol, which leads to the complexity of the technological scheme, the formation of polluted water and waste coal.Closest to the present invention is a method of purifying ethyl alcohol from aldehyde impurities, mainly from acetaldehyde by alcohol treatment at the stage of distillation of the aqueous solution of alkali metal hydroxide  According to the described method, the process of separating ethanol from water-ethanol raw material containing 0,16-0,19 wt. acetaldehyde, carry out multi-stage scheme, which includes the pre-distillation of the lung and the main quantity of aldehydes in the extractive-distillation column, with further diluted to 5.0-10.0 wt. an aqueous solution of ethyl alcohol in the column concentration of allocation of purified ethyl alcohol, at the same time to ensure a high degree of purity of the alcohol in the middle part of the column serves aqueous solution of alkali metal hydroxide. The highest degree of purity alcohol (content of acetaldehyde below 2.0 mg/l) is achieved when the concentration of alkali metal hydroxide in Cuba what about the metal for the chemical binding of acetaldehyde, i.e., a hydroxide of alkaline metal cleaning processes ethyl alcohol is used only for partial binding of acetaldehyde, and the inability to use this method for the purification of alcohol from other carbonyl compounds.The process of purification of ethyl alcohol by treating the alcohol with a mixture of alkali metal hydroxide, taken in an amount of 0.01-0.1 wt. and sodium borohydride in an amount of 0.005 to 0.3 wt. when 30-80aboutWith allows you to get ethyl alcohol of high purity. This method can be effectively used for cleaning contaminated carbonyl compounds concentrated ethyl alcohol by preprocessing the dirty product specified reagents followed by separation of the alcohol by distillation.The upper limit of the concentration of the reagents is limited by the fact that a further increase of hydroxide of an alkali metal higher than 0.1 wt. and sodium borohydride above 0.3 wt. along with providing high purity alcohol only lead to increased consumption of reagents and increasing losses of ethanol on the stage of rectification.The drawing shows a diagram of the proposed installation.Evaluation of the effectiveness DSA the tank 2 for storing contaminated ethyl alcohol, capacity 4 to prepare an aqueous solution of alkali metal hydroxide and sodium borohydride, dosing pumps 3 and 5, the heater 6, distillation column 10, the refrigerator 11, reservoir 12, 13 for collecting the purified ethyl alcohol, the pump 14 for pumping a bottom liquid 15; 1 line input ethyl alcohol, 7, 8, 9 line input of an aqueous solution of alkali metal hydroxide and sodium borohydride.The total content of carbonyl compounds in the source of ethyl alcohol was determined by chromatographic specifications 38.402-62-117-90 using a flame ionization detector. Sorbent diglycerin and polietilenglikolsuktsinata on chromatone, the column length was 3 m, the velocity of the carrier gas 25-30 cm3/min, the temperature of thermostat 55-65aboutWith the temperature of the evaporator 50aboutC. the Content of carbonyl compounds in terms of acetic aldehyde in a purified ethanol depending on their concentration was determined analogizes according to GOST 10749.3-80 and GOST 5964-82.P R I m e R 1 (comparative). Clearing of carbonyl impurities is subjected to synthetic ethyl alcohol conforming to the requirements of THE 38.402-62-117-90 and containing in its composition of 0.14 wt. acetaldehyde, a 0.012 wt. methyl ethyl ketone, 0,009 wt. acetone, 0 prepare a 5.0% solution of sodium hydroxide by filing a 20% aqueous NaOH solution and distilled water. The contaminated alcohol from the tank 2 by the pump 3 with a flow rate of 0.2 l/h is fed through the heater 6 in rectification column. The average length of stay alcohol-flow heater 6 is 1 o'clock Constantly in the contaminated alcohol dosed at 5.0% aqueous sodium hydroxide solution by feeding it the pump 5 to the suction side of pump 3. The consumption of alkali is about 4.0 to 4.5 ml/h and provides the content of sodium hydroxide in an alcohol thread about 0,10-0,12 wt. (analysis of the sampler 16).In the heater 6 liquid stream is heated to 70aboutAnd then enters the distillation column 10 of the Packed type (column filled with a nozzle made of spiral size 2,h,0 mm). Modes of rectification of ethanol following: temperature of top 78,0-78,4aboutTemperatures cube 91-93aboutWith, reflux number of 6.0. CBM product from the column output periodically by the pump 14.Test this mode should be performed within 10 hours as a result providing 1850 purified ethanol: volume fraction of ethyl alcohol to 96.3% of the total carbonyl content in terms of acetic aldehyde 158 mg/lP R I m m e R 2 (comparative). The cleaning process is carried out in the conditions of example 1. Consumption of alcohol 0.2 l/h, GI is from the pump 3. In the heater 6 liquid stream is heated to 70aboutWith, time 1 hThe test results for 10 h emit 1822 alcohol with the following characteristics: volume fraction of ethyl alcohol 96,2% of the total carbonyl content in terms of acetic aldehyde 204 mg/lP R I m e R 3. Cleaning is subjected to synthetic ethyl alcohol of example 1 and test conditions similar to examples 1 and 2. In the vessel 4 is prepared aqueous solution of sodium hydroxide and sodium borohydride containing 2.0 wt. sodium hydroxide and 4.0 wt. sodium borohydride. The resulting solution with a flow rate of 5 cm3/h pump 5 is supplied to the suction side of the pump 3. Consumption of alcohol flow rate of 0.2 l/H. the Content of sodium hydroxide in ethanol stream is 0.05-0.06 wt. and sodium borohydride 0,10-0,12 wt. liquid flow in the heater 6 is heated to 70aboutC. the result of this mode is selected 1836 purified ethyl alcohol with the following characteristics: volume fraction of ethyl alcohol to 96.3% of the total carbonyl content of impurities in terms of acetic aldehyde 1.5 mg/lP R I m e R s 4-12. The cleaning process ethanol is conducted similarly to examples 1-3. During the tests varied the heater 6 in the range of 30-70aboutC.The test conditions and the results obtained are presented in the table.A comparative analysis of the results shows that the process of purification of ethyl alcohol by pre-treatment with a mixture of alkali metal hydroxide and sodium borohydride, taken in an amount of 0.01-0.1 and 0.005-0.3 wt. at a temperature of 30-70aboutWith subsequent isolation of the desired product by distillation provides a high degree of purification of ethanol from a wide range of carbonyl compounds. The decrease in the concentration of these reagents below 0.01 wt. for a hydroxide of an alkali metal and 0.005 wt. for sodium borohydride in the process of purification of the desired result does not.The advantages of this method compared to known are its high efficiency, the need to use simplified process flowsheet absence stages of pre-treatment water, which leads to reduced losses of alcohol and the formation of additional contaminated streams.This method can be used for purifying polluted carbonyl impurities alcohol and processes of ethanol production stages of the separation of the hydroxide of an alkali metal, followed by distillation, characterized in that the treatment is carried out with a mixture of alkali metal hydroxide and sodium borohydride, taken in an amount of 0.01 to 0.1 wt. and 0.005 to 0.3 wt. respectively.
FIELD: chemical industry; method of production of the alkali-resistant and thermal-resistant polyols.
SUBSTANCE: the invention is pertaining to the improved method of production of the alkali- resistant and thermal-resistant polyols representing the sugar-alcohol syrups. The method provides for the following stages: hydrogenation of the hydrolysate of the corresponding polysaccharide with formation of the hydrogenated sugar-alcohol syrup, the alkaline and thermal treatment of the hydrogenated syrup for production of the stabilized sugar-alcohol syrup, refining of the stabilized sugar-alcohol syrup by its gating through, at least, one ion-exchange resin, in which the stabilized sugar-alcohol syrup is refined by means of its double gating through the cationic- anionic ion-exchange configuration (CACA) including, at least, the first weak-acid cationic ion-exchange resin and the second strongly-base, medium-base or weak-base anion-exchanging resin. The method allows to have the alkali-resistant and thermal-resistant polyols not having the shortcomings of the polyols of the previous level of the engineering.
EFFECT: the invention ensures production of the alkali-resistant and thermal-resistant polyols not having the shortcomings of the polyols of the previous level of the engineering.
18 cl, 3 ex, 1 dwg
FIELD: chemical technology.
SUBSTANCE: invention relates to a method for synthesis of 1,3-propanediol involving the following steps: (a) formation of aqueous solution of 3-hydroxypropanal; (b) hydrogenation of 3-hydroxypropanal to form crude mixture of 1,3-propanediol, water and cyclic acetal of molecular mass 132 Da (MW 132 cyclic acetal) and/or cyclic acetal of molecular mass 176 Da (MW 176 cyclic acetal); (c) distillation (drying) of indicated crude mixture of 1,3-propanediol for water removing and formation of the second crude mixture of 1,3-propanediol (the first flow of residues after distillation) containing 1,3-propanediol and MQ 132 cyclic acetal and/or MW 176 cyclic acetal; (d) contact of the flow containing MW 132 cyclic acetal and/or MW 176 cyclic acetal with acid-base cation-exchange resin or with acid zeolite, or with soluble acid, and (e) removal of MW 132 cyclic acetal. Method provides enhancing effectiveness for extraction and purification of 1,3-propanediol.
EFFECT: improved method of treatment.
10 cl, 9 tbl, 1 dwg, 6 ex
SUBSTANCE: invention relates to an improved method of reducing concentration of aldehyde in the crude stream of a carbonylation process, involving feeding a crude stream containing a carbonylatable agent selected from a group consisting of methanol, methyl acetate, methyl formate and dimethyl ether or mixture thereof, having primary concentration of aldehydes; and reaction thereof in gaseous phase with a deposited catalyst which contains at least one metal from group 8 to 11, in conditions which facilitate reduction of primary concentration of aldehydes to secondary concentration of aldehydes.
EFFECT: method improves degree of reduction of aldehyde.
28 cl, 3 tbl, 3 ex
SUBSTANCE: invention relates to a method of improving the quality of ethylene glycol products, where ethylene glycol raw material and hydrogen are fed into a rotary packed bed reactor loaded with a solid oxide catalyst at temperature of about 20 to about 280°C, pressure of about 0.1 to about 4.0 MPa, volume flow rate of about 0.2 to about 100.0 h-1 and hydrogen to ethylene glycol molar ratio of about 0.01 to 40:1, and ethylene glycol is obtained after the reaction, where said solid oxide catalyst is selected from at least one catalyst based on copper, nickel and palladium. The rotary speed of the packed bed reactor ranges from about 300 to about 5000 rpm.
EFFECT: improved quality of ethylene glycol products, specifically high selectivity of trace impurities, which affect transmission of UV radiation for ethylene glycol products, ie achieving a high UV radiation coefficient.
9 cl, 10 ex
SUBSTANCE: claimed invention relates to method for obtaining ethyleneglycol from ethylene. Method includes the following stages: i) transformation of ethylene into ethylenoxide in presence of oxygen, catalyst of epoxidation and retardant in ethylenoxide reactor; ii) absorption of ethylenoxide with absorbent water solution and the following stripping of said absorbent to obtain flow of ethylenoxide water solution; iii) transformation of flow of ethylenoxide water solution into ethylenecarbonate flow in presence of one or several catalysts and carbon dioxide in one or several reactors of carboxylation; iv) transformation of ethylenecarbonate into first ethyleneglycol flow in presence of one or several catalysts in one or several hydrolysis reactors; v) removal of water from first ethyleneglycol flow to obtain dehydrated ethyleneglycol flow and wasted water flow in one or several dehydration columns; vi) purification of dehydrated ethyleneglycol flow in one or several ethyleneglycol distillation columns to obtain flow of purified ethyleneglycol product and recirculation catalyst flow. First ethyleneglycol flow contains inorganic chloride admixtures, and method includes the following additional stages: vii) transformation of inorganic chloride admixtures into 2-chloroethanol by reaction with ethylenoxide in one or several dehydration columns and viii) removal of 2-chloroethanol in wasted water flow.
EFFECT: claimed method makes it possible to reduce or eliminate necessity in catalyst discharge.
10 cl, 2 dwg, 1 tbl, 1 ex
FIELD: distillery industry; production of a dehydrated ethyl alcohol.
SUBSTANCE: the invention is pertaining to the field of distillery industry, in particular, to the methods of production of a dehydrated ethyl alcohol. The method provides for concentration of the water-alcohol solution purified from impurities by a rectification, its dehydration by adsorption through the molecular sieves and its regeneration by a desorption. Concentration of the water-alcohol solution and its dehydration by adsorption are conducted at the pressure of 105-350 kPa. A part of the formed during the concentration vapors is once more heated up to the temperature of 96-150°C and feed to the stage of desorption, which is realized at the pressure of 5-60 kPa. The rest part of the vapor from the stage of adsorption and a desorption is subjected to condensation and the water-alcohol liquid is fed to the stage of the alcohol concentration with withdrawal of the water from the process. The invention allows to intensify the process of dehydration and to reduce consumption of the heat-power input.
EFFECT: the invention allows to intensify the process of dehydration and to reduce the heat and power inputs.
FIELD: method for production of alcohol-containing solvents based on waste from ethanol production from food-grade raw materials.
SUBSTANCE: claimed method includes reprocessing of etheraldehyde fraction of concentrate containing ethanol main admixtures from starch- and/or sugar-containing raw materials. Process is carried out in rectifier at vapor phase temperature in still of 60-90°C. Nitrosolvent is obtained by mixture sampling at 60-70°C. Degreasing solvent is obtained by mixture sampling at starting temperature in column top of 73°C or more when ethers are detected in distillate. Claimed nitrosolvent (degreasing solvent) contain (mass %): acetate-type ethers 10-30 (0.8-2.9); aliphatic alcohols 51-74 (87-89); acetaldehyde 5-9 (0.2-1.5), and water 8-10 (8-10).
EFFECT: simplified and economy method for reprocessing of waste from ethanol production; enhanced assortment of alcohol-containing solvents.
3 cl, 1 dwg, 3 ex, 3 tbl
FIELD: alcohol production.
SUBSTANCE: method comprises direct distillation of concentrate of top ethyl alcohol impurities or rectification of intermediate ethyl alcohol fraction in presence of an alkali agent selected from sodium and potassium oxide, carbonate, and bicarbonate hydrates, and aqueous ammonia in case of top ethyl alcohol impurities processing and selected from sodium and potassium oxide, carbonate, and bicarbonate hydrates, calcium oxide, and aqueous ammonia in case of intermediate ethyl alcohol fraction rectification at alkali agent concentration 0.01 to 3.0 wt % and vat temperature 80-86°C. Desired processing product is commonly used as a binary mixture component and vat residue obtained in distillation and rectification operation is commonly used as additional component of fuel oil.
EFFECT: achieved wasteless processing of alcohol production wastes and utilization of all processing products.
FIELD: industrial organic synthesis and chemical engineering .
SUBSTANCE: invention relates to a process of producing liquid oxygenates, including methanol, C2-C4-alcohols, formaldehyde, lower organic acids, or mixtures thereof, and to installation for implementation the process. Process comprises successively supplying natural gas from complex gas preparation plant to a series of "gas-gas" heat exchangers and into annular space of at least one tubular reaction zone of reactor, wherein natural gas is heated to temperature of the beginning of reaction, whereupon heated gas is passed to the entry of the tubular reaction zone mixer, into which compressed air or oxygen is also injected to provide gas-phase oxidation in reaction zone of reactor. Resulting reaction mixture is discharged from reactor into a series of "gas-liquid" and "gas-gas" heat exchangers, wherein reaction mixture is cooled to ambient temperature and sent to separator, wherefrom liquid phase is passed through lower carboxylic acid recovery vessel to the system of rectification columns to isolate the rest of mixture components, whereas leaving gas is recycled to complex gas preparation plant. More specifically, oxidation is carried out within temperature range 240 to 450°C and pressure from 2 to 10 MPa at residence time of reaction mixture in reactor 2-6 sec and oxidant concentration 2 to 15 wt %. In reactor having mixers hollow and at least one tubular reaction zones, required temperature is maintained constant throughout all length of tubular reaction zone and at entries for compressed air or oxygen in mixers of each of tubular reaction zones and hollow reaction zone. Liquid oxygenate production plant is composed of aforesaid complex gas preparation plant, a series of "gas-gas" heat exchanger to heat natural gas, reactor, a series of "gas-liquid" and "gas-gas" heat exchangers to cool reaction mixture obtained in reactor, gas-liquid separator, lower carboxylic acid recovery vessel, and system of rectification columns to isolate the rest of products.
EFFECT: enabled implementation of the process directly near gas and gas condensate deposits, increased conversion of methane per one passage through reactor, and increased yield of oxygenates due to improved design of plant.
6 cl, 1 dwg, 1 tbl
SUBSTANCE: invention pertains to the method of oxidation of hydrocarbons using oxygen in trifluoroacetic acid and can be used particularly for oxidation of alkanes, cycloalkanes, alkylaromatic hydrocarbons, alkenes, cycloalkenes. The method involves saturation of trifluoroacetic acid with oxygen, after which, the initial hydrocarbon is added to the obtained reaction medium and is kept until depletion of bound oxygen with obtaining the corresponding oxygen containing compound.
EFFECT: invention allows carrying out a process of selective partial catalytic oxidation of hydrocarbons with obtaining different oxygen containing organic compounds without use of high temperature and traditional catalyst systems based on transition metals.
1 tbl, 5 ex
FIELD: food products; alcoholic beverages.
SUBSTANCE: according to the method, initial flow is supplied to the first distillation steam-stripping column while its distillate is passed to the second distillation rectifying column. Initial flow is refined using first membrane separation method. Obtained concentrate is passed to the first distillation column and derived permeate is supplied to the second distillation column. Distillate from the second distillation column is refined using second membrane separation method.
EFFECT: increasing pureness of obtained ethanol.
16 cl, 2 dwg, 2 tbl
SUBSTANCE: method of processing carbon-carbonate mineral involves burning limestone in a reactor, obtaining calcium oxide, production of calcium carbide by reacting part of calcium oxide obtained from burning limestone with carbon, bringing part of the obtained calcium carbide into contact with water, obtaining acetylene and caustic lime, bringing gaseous wastes from burning limestone into contact with water to obtain carbonic acid. Limestone is burnt using heat obtained from burning part of the volume of acetylene, obtained from part of the volume of calcium carbide. At least part of the obtained acetylene is used in synthesis of ethanol and/or dichloroethane and/or ethyleneglycol and/or acetone. During synthesis of ethanol and/or dichloroethane, acetylene is reacted with hydrogen in the presence of palladium as catalyst, after which at least part of synthesised C2H4 material is reacted with water vapour, obtaining ethanol, and/or reacted with chlorine, obtaining dichloroethane. Also at least part of the obtained acetylene is subjected to hydrolysis, obtaining ethyleneglycol. Also during synthesis of acetone, part of the obtained acetylene is reacted with water vapour, where the hydrogen obtained is used in said synthesis of ethanol and/or dichloroethane and/or burnt in the burning process. Carbon dioxide obtained from synthesis of acetone is used in the process of producing carbonic acid.
EFFECT: wide range of obtained finished products and prevention of formation of industrial wastes.
4 cl, 1 ex, 1 dwg
SUBSTANCE: present invention relates to a method of processing alcohol production wastes: concentrate of head impurities of ethyl alcohol (CHI) and an intermediate fraction of ethyl alcohol (IFEA). The method involves obtaining a water-alcohol solution of CHI or IFEA with density (0.837-0.940) g/cm3 (I) and conducting continuous extraction of impurities (C3-C5 alcohols, esters, carbonyl compounds) in a packed column with a mixture of aromatic hydrocarbons (II) or a mixture of aromatic and aliphatic hydrocarbons (III) with ratio of volume flow I: II or, respectively, I : III, equal to 1:(1-4) (preferably 1:1.2). To intensify mass exchange into solution (I), (0.1-0.5) wt % mixture (IV) of anionic alkyl sulphates and noionic oxyethylated alkyl phenols in ratio (25-20):(70-75) wt% (IV). The desired processing products: raffinate - aqueous of ethanol with weight ratio of the latter equal to (80-20) wt % can be used to obtain high-purity edible ethyl alcohol and as an anti-icing agent for glass used on cars, and extract - solution of alcohol and esters in a mixture of hydrocarbons is used to prepare mixed solvents for the paint industry.
EFFECT: high efficiency of the method of processing alcohol production wastes.
4 cl, 8 ex, 1 tbl, 2 dwg
SUBSTANCE: method involves partial oxidation of an alkane contained in a gaseous crude stream, which contains an alkane, with oxygen contained in an oxygen-containing crude stream. Said method involves: forming a reactor system, having a back-mixing reaction chamber with injection mixing, which is connected to a tubular flow reactor, wherein said back-mixing reaction chamber with injection mixing ensures dwell time from about 0.05 s to about 1.5 s; feeding said crude stream containing alkanes and said oxygen-containing crude stream into said back-mixing reaction chamber with injection mixing; initiating formation of alkyl free radicals in said back-mixing reaction chamber with injection mixing to obtain a product stream from the back-mixing reaction chamber with injection mixing, containing oxygen, said alkane and at least a portio of said alkyl free radicals; feeding the product stream obtained in the back-mixing reaction chamber with injection mixing into the tubular flow reactor; and converting said product stream obtained in the back-mixing reaction chamber with injection mixing into said alkyl oxygenate in said tubular flow reactor; where said alkane is selected from group consisting of methane, ethane, propane and butane.
EFFECT: invention enables to obtain the end product using an efficient and cheap method without using a catalyst.
34 cl, 2 ex, 36 dwg
SUBSTANCE: present invention relates to a method of producing dehydrated ethyl alcohol, which can be used in chemical, electronic and pharmaceutical industry. The method involves feeding crude alcohol or a water-alcohol solution into a preliminary dehydration column operating under a vacuum to obtain a distillate which is fed into a final dehydration column operating at excess pressure, where dehydrated alcohol is collected in form of a residue and the distillate is fed into the preliminary dehydration column in form of reflux. The distillation process in the preliminary dehydration column takes place at absolute pressure of 8.0-13.3 kPa to obtain a distillate with alcohol content 98.2-98.9 vol. %, and the distillation process in the final dehydration column takes place at absolute pressure 0.1-0.5 MPa and alcohol content in the reflux of 96.5-97.2 vol. %.
EFFECT: method enables to obtain an end product of high quality using an improved an improved process scheme.
1 tbl, 1 dwg, 2 ex