The isolation and purification of secondary butyl alcohol

 

(57) Abstract:

Usage: basic organic synthesis. The inventive product is secondary butyl alcohol, B. F. Sanyo, the concentration of 70%. The method of selection of co - CiOHi in Hume, Mio fluid., .,,. mukti dehydration TBS sent to the reactor-rectifier , in the upper part of which is placed a layer of ion-exchange catalyst. The process of concentration and purification VBS conducted at temperatures top 85-PS and the temperature of the cube reactor 95 P°C at a pressure of 0.01 to 0.02 MPa 1 table

 

Same patents:

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to improved process of high-purity solvent-grade fluorinated alcohol production, which comprises reaction of methanol with tetrafluoroethylene or hexafluoropropylene in presence of alkylperoxide. Process leads to formation of fluorinated alcohol having general formula: H(CFR1CF2)nCH2OH (I), wherein n=1 or 2; when n=1, R1 represents F or CF3 and, when n=2, R1 represents F. After completion of reaction, reaction mixture is distilled on distillation column in presence of water and HF to produce (i) top fraction containing alcohol formed from alkyl peroxide, water, and HF and (ii) bottom liquid containing fluorinated alcohol of formula (I). Bottom liquid is purified to recover desired fluorinated alcohol.

EFFECT: increased yield of product.

7 cl, 3 dwg, 2 ex

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.

6 cl

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to improved process for production of 2-ethylhexanal, which is raw material for production 2-ethylhexanoic acid and/or 2-ethylhexanol. Starting material of invention is bottom residue from rectification of butyl alcohols produced in oxo synthesis, from which bottom residue a fraction mainly containing saturated and unsaturated C8-alcohols with 5-15% of C12-acetals is isolated on two columns operated at column top residual pressure 50-90 mm Hg. This fraction is subjected to vapor-phase processing at atmospheric pressure on copper-containing catalyst at 200-300°C followed by rectification of catalysate on two columns to isolate, as first-column top distillate, fraction obtained at 20-50 mm Hg and containing light components and 2-ethylhexanal, which fraction is fed into second column operated at column top residual pressure 60-100 mm Hg to isolate distilled fraction containing light components and 30-60% of 2-ethylhexanal, whereas desired 2-ethylhexanal is recovered as bottom product or as product tapped from the side of bottom column section.

EFFECT: improved quality and yield of desired product.

2 cl, 14 ex

FIELD: petrochemical industry; methods of production of ethylene chlorohydrin.

SUBSTANCE: the invention is pertaining to the field of petrochemical industry, in particular, to the method of the vacuum rectifying separation of ethylene chlorohydrin (EChH) both from the mixtures with the high-boiling hydrins and at the regeneration of EChH in the process of the synthesis of the different compounds on its base. The method provides for the vacuum rectification of EChH with the continuous feeding of ethylene oxide into the distillation residue section of the column of separation up to its content in the distillation residue liquid within the interval of 0.01-0.15 mass % at the temperatures exceeding 90°C. As a rule the ethylene oxide is introduced in the form of the solution in the material flow of the phase of the rectification. The method ensures reduction of the corrosion activity of the medium, the increased reliability and the service life of the equipment, stabilization of the commercial EChH quality and the raised efficiency.

EFFECT: the invention ensures reduction of the corrosion activity of the medium, the increased reliability and the service life of the equipment, stabilization of the commercial EChH quality and the raised efficiency.

2 cl, 1 tbl, 9 ex

FIELD: rectification of organic compounds.

SUBSTANCE: all-purpose installation enables purification of high-boiling vacuum rectification solvents, in particular ethylene glycol, monoethanolamine, methyl cellosolve, ethyl cellosolve, butyl cellosolve, N-methylpyrrolidone, and benzyl alcohol.

EFFECT: enhanced purification efficiency.

8 cl, 1 dwg, 7 tbl, 7 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention provides a method for purifying 1,3-propanediol comprising: (a) optional removal of water from raw mix containing 1,3-propanediol; (b) distillation of raw mix containing 1,3-propanediol in distillation column under conditions favoring maximum separation of mix components, which are heavier than 1,3-propanediol, from 1,3-propanediol and components, which are lighter than 1,3-propanediol; (c) withdrawal of stream containing at least major part of 1,3-propanediol and at least some components, which are lighter than 1,3-propanediol; (d) separation of stream from step (c) from components, which are heavier than 1,3-propanediol; and (e) distillation of stream from step (c) in distillation column to separate 1,3-propanediol from components of stream, which are lighter than 1,3-propanediol, and any residual components heavier than 1,3-propanediol.

EFFECT: enhanced purification efficiency.

10 cl, 3 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of separating a solution of homogeneous catalyst from unrefined monoethylene glycol (MEG) and purifying MEG, for use in catalytic conversion of ethylene oxide (EO) to MEG, where the method involves the following steps: separating the catalyst solution in a catalyst separation section by evaporating unrefined MEG and feeding the unrefined MEG into a rectification section, a section for separating light fractions and from there into a pasteurisation section, where each section works at pressure lower than atmospheric pressure of 0.5105 Nm-2 or lower, where the rectification and pasteurisation sections are at pressure lower than that of the catalyst separation section, where the method provides pressure difference between the catalyst separation section and the rectification section, and where the vapour phase of the unrefined MEG from the catalyst separation section is fed essentially as vapour-phase feed into the rectification section. The invention also relates to apparatus where said method can be realised, as well as use of said method and apparatus in a process or block for catalytic conversion of EO into MEG.

EFFECT: invention enables to reduce the process to a one-run process of evaporating a stream of monoethylene glycol, which enables to transport vapour from the catalyst separation section into the monoethylene glycol purification step without using a mechanical pump.

12 cl, 3 dwg

FIELD: explosives.

SUBSTANCE: method to produce isopropanol is carried out in process of at least two reaction stages of hydrogenation, at the same time each reaction stage includes a reaction zone of hydrogenation, where the hydrogenation product released from the reaction zone of the first reaction stage contains a non-reacted acetone, and a flow of products containing acetone and isopropanol is supplied into the reaction zone of the next reaction stage, at the same time the specified flow of products at the inlet to the reaction zone of the specified next stage has temperature from 60 to 100C. At the same time the temperature of the flow of products released from the reaction zone of the specified next reaction stage, at the outlet of the specified reaction zone is at least by 40C higher than the temperature of the flow of products arriving into the specified reaction zone at the inlet to the specified reaction zone, and the temperature in the specified next reaction zone does not exceed 125C.

EFFECT: method makes it possible to produce isopropanol of high degree of purity.

23 cl, 2 ex, 1 tbl, 1 dwg

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing rectified ethyl alcohol and apparatus for realising said method. The method involves distillation of alcohol and attendant impurities in a mash column, purification of alcohol from head impurities in an epuration column, concentration of alcohol and purification thereof from intermediate impurities and residues of heat impurities in an alcohol column, and separation of impurities in a column for concentration of head and intermediate impurities. The wash distillate is fortified in the concentration part of the mash column; extraction of impurities in the epuration column is carried out with intense feeding of hot water for hydro-selection into the top tray and the middle part of the epuration column; purification of alcohol from methanol is carried out in a methanol column; lutter water from the alcohol column is fed into the top tray and the middle part of the column for concentration of head and intermediate impurities; lutter from the column for concentration of head and intermediate impurities is fed into the top tray and the middle part of the epuration column.

EFFECT: invention enables to obtain ethyl alcohol of high quality with minimum loss thereof with by-products.

2 cl, 1 tbl, 1 dwg

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

FIELD: chemistry.

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

FIELD: chemistry.

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 280C, 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

FIELD: chemistry.

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: organic chemistry, in particular production of high oxoalcohols.

SUBSTANCE: invention relates to method for production of high oxoalcohol from isomeric olefin mixture containing from 5 to 24 of carbon atoms. Claimed method includes hydroformylation in presence of catalyst at elevated temperature and elevated pressure. Hydroformylation in carried out in one step, and ones-through olefin conversion is limited in range of 40-90 %. Obtained reaction mixture after catalyst separation is preferably transferred to selective hydration carrying out at 120-220°C and pressure of 5-30 bar in presence of supported catalyst containing copper, nickel and chromium as active ingredients. Hydration product mixture is separated by distillation, and olefin fraction is recycled into hydroformylation step. As starting materials for hydroformylation mixtures of C8-, C9-, C12- or C16-olefins are used.

EFFECT: high olefin conversion ratio, selectivity, and capability.

15 cl, 1 dwg, 1 tbl, 2 ex

FIELD: petrochemical industry; methods of hydrocarbon mixtures refining.

SUBSTANCE: the invention is pertaining to the field of petrochemical industry, in particular, to refining of the hydrocarbon mixtures. The invention provides for refining of a hydrocarbon mixture containing iso- and normal butanes and, probably, the butanes containing as a minimum two stages of the contacting with the solid high-acidic catalyst(s). The mixture first is exposed to refining at the stage(-s) mainly of the primary transformation of isobutene: from the product(-s) distil off a mixture of the non-reacted hydrocarbons C4, which then is exposed to a liquid-phase refining at the stage(-s) of the primary transformation of n-butanes and from the product distil off the non-reacted hydrocarbons containing predominary butanes. At the stage(-s) of the primary transformation of isobutene the contacting is carried out at the presence of water and-or alcoholC1-C2 in a quantity sufficient for transformation of the majority of isobytene into tret-butanol and-or into alkyl-tret-butyl ether. At the stage of primary transformation of n-butenes feed the mixture of the non-reacted hydrocarbons containing no more than 8 % of isobutene and admixture of water and-or alcohol from a previousa stage (-s) and the majority of n-butenes transform into dimers and codimers of n-butenes at the temperature of as a minimum by 15°C higher, than at the stage(-s) of the primary transformation of isobutene. The technical effect: transformation of the tret-alkenes into the oxygen-containing products having the high octane numbers.

EFFECT: the invention ensures transformation of the tret-alkenes into the oxygen-containing products having the high octane numbers.

11 cl, 2 tbl, 4 ex

FIELD: petrochemical processes.

SUBSTANCE: alcohols such as tert-pentanol or tert-butanol are obtained via liquid-phase hydration of alkenes contained in hydrocarbon feedstock in presence of solid high-acidity catalyst at elevated temperature in two consecutive stages followed by separation of unreacted hydrocarbons from reaction mixture withdrawn, preferably via rectification, from the second stage and containing synthesized alcohols. In the first reaction stage carried out at higher temperature, reaction zone(s) comprises two liquid phases, of which phase containing basically water, is in essential weight excess and phase mainly containing hydrocarbon(s) is in dispersed state. Withdrawn is only or mostly (i) liquid stream containing mainly hydrocarbon(s), synthesized alcohol(s), and dissolved water and optionally (ii) liquid stream containing basically water and alcohol(s). The latter, in the second stage, is fed through distribution device(s) into one or several in series arranged reaction zones, water being introduced into one or several reaction zones separately, and liquid in the second-step reaction zones, operated at lower temperature, is maintained in homogenous or heterogeneous state wherein one phase containing basically water and alcohol(s) is in dispersed state and its weight does not exceed 25% of the weight of phase basically containing hydrocarbons and alcohol(s).

EFFECT: increased conversion of feedstock and accelerated reaction.

12 cl, 1 dwg, 3 tbl, 6 ex

FIELD: petrochemical processes.

SUBSTANCE: alcohols such as tert-pentanol or tert-butanol are obtained via liquid-phase hydration of alkenes contained in hydrocarbon feedstock in presence of solid high-acidity catalyst at elevated temperature in two consecutive stages followed by separation of unreacted hydrocarbons from reaction mixture withdrawn, preferably via rectification, from the second stage and containing synthesized alcohols. In the first reaction stage carried out at higher temperature, reaction zone(s) comprises two liquid phases, of which phase containing basically water, is in essential weight excess and phase mainly containing hydrocarbon(s) is in dispersed state. Withdrawn is only or mostly (i) liquid stream containing mainly hydrocarbon(s), synthesized alcohol(s), and dissolved water and optionally (ii) liquid stream containing basically water and alcohol(s). The latter, in the second stage, is fed through distribution device(s) into one or several in series arranged reaction zones, water being introduced into one or several reaction zones separately, and liquid in the second-step reaction zones, operated at lower temperature, is maintained in homogenous or heterogeneous state wherein one phase containing basically water and alcohol(s) is in dispersed state and its weight does not exceed 25% of the weight of phase basically containing hydrocarbons and alcohol(s).

EFFECT: increased conversion of feedstock and accelerated reaction.

12 cl, 1 dwg, 3 tbl, 6 ex

FIELD: industrial organic synthesis.

SUBSTANCE: invention relates to production of butyl alcohols via oxo synthesis, which comprises propylene hydroformylation stage using cobalt carbonyls as catalyst; distilling off butyric aldehyde concentrate containing, in addition to butyric aldehydes, butyl alcohols, water, unsaturated and saturated dibutyl ethers, butyl formates, butyl butyrates, hydrocarbons, aldehydes and alcohols C-8, C12-acetals, and other high-boiling by-products; and liquid-phase hydrogenation of above concentrate on alumino-zinc-chromium catalyst at 280-320°C and pressure 240-300 kg/cm2 followed by recovering commercial isobutyl and n-butyl alcohols from resulting hydrogenate by rectification of six columns. The latter stage comprises: isolation of unreacted butyric aldehydes, methanol, water, and hydrocarbon traces from top part of first column; passing bottom product of the first column into second column and isolation of butyl alcohols with traces of unsaturated and saturated dibutyl ethers from top part of second column; passing bottom product of the second column into third column and isolation of residual butyl alcohols from top part of third column operated at residual pressure 40-400 mm Hg; passing second-column distillate into fourth column and isolation of crude isobutyl alcohol from top part of forth column and crude butyl alcohol from bottom part of the same column. Commercial isobutyl alcohol is obtained on fifth column and commercial butyl alcohol on sixth column. Furthermore, hydrogenation raw mix is supplemented by mixture of water and third-column distillate fraction 140-170°C at weight ratio (0.3-4.0):1, respectively, so that summary concentration of water in hydrogenation raw mix is maintained between 2.0 and 6.0 wt %.

EFFECT: increased yield of butyl alcohols.

8 ex

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

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