Method of fractionation of multi-component mixtures and device for realization of this method

FIELD: separation of multi-component mixtures; chemical, pharmaceutical, oil-and-gas refining and food-processing industries; treatment of sewage.

SUBSTANCE: proposed method is based on continuous counter-flow of liquid and gaseous components excluding mixing of phases at continuous removal of gaseous and liquid components from column. Column is located at angle of 5-10° and is filled with glass balls, 1-6 mm in diameter by 1/2-2/3 of volume. Process is continuous at simultaneous regeneration of all components.

EFFECT: reduced energy requirements; reduced usage of metals; low cost of finished product.

5 cl, 1 dwg, 5 ex

 

The invention relates to methods and devices for the separation of multicomponent mixtures and can be used in chemical and pharmaceutical, oil and gas processing and food industries, as well as for industrial wastewater treatment. Now for the fractionation of multicomponent mixtures of known composition on an industrial scale using different distillation columns.

Known methods for separation of multicomponent mixtures based on differences in physico-chemical properties of the mixture components, for example, the boiling temperature [1, 2], or on differences in chemical properties [3]. However, the known methods have some disadvantages, namely:

1. The need for translation into the vapor state of the total weight of the solution and, consequently, high energy intensity.

2. It is difficult practionercourse components with similar boiling points or chemical properties.

3. The sequence of selection of the components of a mixture in order to modify the chemical or physico-chemical properties.

4. The need for disposal or regeneration of the sorbent and additionally separated by.

5. Slow speed fractionation.

The closest techniques are methods of separation of mixtures on the medicinal components, including the use of chromatographic columns. However, these methods have the following problems is ADI:

1. The sorbent is used only for additional cleaning vapor mixture before it is fed to the rectification [patent RU 2057797, 1996].

2. Separation of the mixture components in a chromatographic column occurs in the fluidized bed, which requires the presence of recirculation pump regulating pressure in each section of the column [patent RU 2143941, 1995].

The present invention is to develop a method of fractionation of multicomponent mixtures, eliminating the disadvantages of the known methods, allowing simultaneous selection of all the components of the mixture. The problem is solved in that a method for fractionation of multicomponent mixtures based on continuous countercurrent liquid and gaseous components, excluding the mixing phase with continuous removal of gaseous and liquid components from the column. For carrying out the proposed method the proposed device. Currently known methods of fractionation of multicomponent mixtures containing vertical distillation or chromatographic columns, which, in addition to the above a number of disadvantages:

1. The difficulty scaling.

2. Long-term regeneration of all components of the mixture has a high cost, which is reduced only if tonnage output.

3. High metallic the efficiency of the equipment.

4. The difficulty of operating in tonnage production.

The technical result to be obtained by use of the invention is:

1. Continuity fractionation.

2. Simultaneous regeneration of all the components of the mixture.

3. Low-intensity, metal consumption and floor space demand.

4. Ease of scale - from installations for scientific research to tonnage production.

5. Reducing the cost of regeneration of the sorbent and the absence of additionally separated by.

6. The horizontal placement of the columns.

7. The potential use of technology in various industries.

8. Reliability at an average level of qualification of the staff.

9. Low cost of the installation and its components. For carrying out the proposed method the proposed device for fractionation of multicomponent mixtures (see)containing tank (1) with a device to maintain a constant level of the solution and ensure a continuous flow of solution in the column for fractionation (2-6). The latter consists of a series of sections arranged at an angle of 5÷10° in the form of "bunching", the number of which is equal to either the amount of the mixture components or group of components. Within each section in its lower the Asti are teploelektronagrevatel (Tans), heating the solution in this section, up to the boiling temperature of a particular component of the mixture with increasing heating temperature of each subsequent section in the downward direction. Each section containing insulating layer is a hollow tube filled with1/2÷2/3their volume of glass beads with ⊘=1,0÷6.0 mm, located around the heating Elements, the surface of which is chemically modified alkyl(aryl)silanes or silane containing chelating agents, resulting in chromatography of the mixture with simultaneous evaporation of components in a continuous mode. Vaporous products are moving up due to the angle on top, free from glass beads to the volume removed through the top opening of the column and are condensed in the refrigerator. The solution flows down the volume filled with glass balls through the same angle, and is removed from the column through the bottom hole. As a result, the column shall countercurrent gaseous and liquid products without stirring.

The claimed device operates as follows. Open the valve for feeding the mash tank (not shown) in tank No. 1. After filling the tank, open the valve on the bottom of the drain to feed the mash in the heated column at a certain speed the flow is. On the remote control turn up the heat all columns in the specified mode and open the taps to supply water in the refrigerator. After the temperature of the columns on the regime begin to collect the products of fractionation in appropriate containers: ethanol fraction in the tank # 14, the light fraction in the tank # 13, fusel oil in the tank # 11. Further, the unit operates in automatic mode.

Thus, the set of essential features provides getting a new technical result, which is in a continuous fractionation of multicomponent mixtures with simultaneous separation of all components in the horizontal column, filled with sorbent with a chemically modified surface for long time operation without regeneration of the sorbent; in reducing its energy and metal consumption, production costs and production facilities, the ability to use technology in different industries and at different scales, i.e. the essential features are in causal relationship with the specified technical result.

EXAMPLE 1.

The use of the claimed invention in the production of ethanol qualification "Food".

The mash tank (1) continuously by gravity in the heated column (2), completely filled glass the balls with ⊘ =2±0.2 mm, where it is heated by the Heater to t=70±2°S. Of heated columns mash continuously by gravity in the first section (3) of the column for fractionation, which1/2÷2/3its volume filled glass bulbs ⊘=2±0,2 mm Solution in this column is heated by the Heater to t=75±1°C. At this temperature from the mash continuously distills components with a boiling point below 75°and their subsequent condensation in the refrigerator (4). Then mash continuously by gravity in bragadireanu column, consisting of three sections (5÷7)filled in1/2÷2/3volume of glass beads with ⊘=4±0,2 mm Solution in all sections is heated by the Heater up to t=80±2°C. Vapors of ethyl alcohol derived from each section through the upper hole and sent either in a refrigerator (8) to obtain a crude alcohol or firming column (9), and the solution fusel oil continuously flows or in a refrigerator (10) and then into the collection (11) or, bypassing refrigerator, hot is directed to a similar installation for the initial removal of water and subsequent fractionation of fusel oils components. Firming column filled with1/2÷2/3volume of glass beads with ⊘=2±0,2 MMARY ethyl alcohol from the strengthening of the column through the top hole is continuously output in the fridge (12), then the collection (13), and the solution is returned to in section (7) for the distillation of ethanol.

The claimed device can work in combination with a device for continuous generation of brew from sugar mash with the use of chemically immobilized yeast on glass beads or pure cellulose.

EXAMPLE 2.

The use of the claimed invention in pharmaceutical production.

In the manufacture of pharmaceutical preparations "Mebicar" and "Albacar" getting pharmacopoeial substance of the product is carried out by recrystallization from ethanol. Alcohol solution after separation from it pharmacopoeial product is directed to the regeneration of alcohol in the convoy, consisting of two sections. The first section (heating) is completely filled with glass beads with ⊘=2±0.2 mm, where the solution is heated by the Heater to t=75±1°and the second section (alcohol-distillation) filled with glass balls on1/2÷2/3volume and is heated by the Heater up to t=80±2°C. a Pair of ethanol through the top hole is removed from the column, condensed in the condenser and returned to the production cycle at the stage of recrystallization, and the VAT residue on stage freezing pharmacopoeial product.

In this pharmaceutical production the La allocation technical product from the reaction mixture used chloroform, which is extracted drugs. The selection of the technical product from a solution of chloroform is carried out on a similar setup, only the heating temperature of the column correspond to the boiling point of chloroform.

EXAMPLE 3.

Use the claimed invention in the oil and gas industry.

In the production of motor fuels at refineries are formed gaseous products, which are burned in flares. For the elimination stage of combustion of the gaseous products of the latter are sent to fractionation on a column consisting of a number of sections equal to the number of components of the gas mixture. Columns filled with ethyl alcohol and glass beads with ⊘=4-6 mm, whose surface is chemically modified by alkylsilane, for example, trebujena. The gas flow of hydrocarbons, passing through all the sections of the column, due to different solubility in ethyl alcohol and the length of the alkyl radical of a hydrocarbon is divided in sections (chromatographies) in descending order of the number of carbon atoms in the alkyl radical. Absorption of gaseous hydrocarbons ethyl alcohol is carried out at room or low to 5÷10°With temperature, owing to external cooling. After reaching the saturation point of ethanol hydrocarbon gas n the current is directed in a parallel column, and in the first column of each section is heated by a Heater located inside the column, to a certain temperature, after which the solution is removed hydrocarbons and does not evaporate the alcohol. Then the column is cooled and the cycle repeated fractionation.

With this method instead of the traditional method of fractionating the liquid hydrocarbons formed by cracking oil, practionercourse on the column, consisting of a number of sections corresponding to the number of hydrocarbon groups with close (within 5-10° (C) boiling temperature. Section filled with1/2÷2/3volume of glass beads with ⊘=4÷6 mm, whose surface is chemically modified alkyl(aryl)silanes. Evaporated in each section of the hydrocarbons are condensed in a separate refrigerators and are independent commodity product or mixed in certain proportions to achieve the desired octane number motor fuels.

EXAMPLE 4.

The use of the claimed invention for the treatment of industrial wastewater and waste chemical and chemico-pharmaceutical industries.

Treatment of industrial wastewater is carried out in the columns containing the number of partitions corresponding to the number of impurities. Section columns are heated by heating Elements and filled with1/2÷2/3obamascare balls with ⊘ =4÷6 mm beads Surface in some sections of chemically modified silanes containing chelating agents for water treatment to remove inorganic impurities. As in other sections - silanes with functional groups for water purification from organic impurities. The chemical composition of silane is chosen individually in each case under the chemical composition of the impurities. Impurities after their removal from the wastewater is returned to the process cycle. The device operates in continuous mode with a capacity corresponding to the volume of wastewater particular company.

EXAMPLE 5.

The use of the claimed invention for the treatment of drinking water.

Water from the reservoir after stage flocculation and coagulation pre-cleared in accordance with example No. 4. To achieve the requirements of GOST [4] on drinking water it arrives at the treatment in the claimed device, consisting of columns, which is filled with glass beads with ⊘=1÷2 mm, whose surface is chemically modified with silanes containing chelating agents with cationic or anionic activity. After purification of water from inorganic impurities it is additionally directed to a bactericidal treatment.

References

1. Him, Aouina. Waste biotechnology of ethanol.- M.: Energoatomizdat, 2001, p.69-107.

2. D. Adler, And Nechvatal, Ajutb "Industrial organic chemistry".- M.: Mir, 1977, s-134.

3. The chromatography. Practical application of the method. Ed. E. Heftman, in 2 parts, edited Ph.D. Professor Wegerzyn, M.: Mir, 1986

4. Gstmi.: Water. Control of chemical, bacterial and radiation safety according to international standards. Encyclopedic Handbook, 3rd edition. CJSC "OST-AQUA" and Chernogolovka.

1. Method of fractionation of multicomponent mixtures based on continuous heating and counterflow of liquid and gaseous components, excluding the mixing phase with continuous removal of gaseous and liquid components from the column located at an angle of 5÷10° and filled with 1/2÷2/3 of the volume of glass beads with ⊘=1÷6 mm

2. The method according to claim 1, characterized in that the glass beads chemically modified alkyl(aryl)silanes.

3. The method according to claim 1, characterized in that the glass beads chemically modified silanes containing chelating agents with cationic and anionic activity.

4. Device for fractionation of multicomponent mixtures containing the tank for the mixture, heating the column, the column for fractionation, consisting of several sections arranged at an angle of 5÷10° and filled with 1/2÷2/3 of the volume of glass beads with⊘ =1÷6 mm, an external insulating layer teploelektronagrevatel elements within sections interconnected in the form of "bunching", with branches for removal of gaseous products and refrigerators for condensation of the above sections, containers for collection of end-products, remote control.

5. The device according to claim 4, characterized in that column for fractionation has external cooling.



 

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FIELD: wine-making industry.

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EFFECT: improved manufacturing method.

3 cl, 3 ex

The invention relates to the wine industry and can be used at home

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2 cl, 4 ex, 10 tbl, 5 dwg

FIELD: distillery industry; production of alcohol.

SUBSTANCE: the invention presents a method of production of a rectified alcohol and is dealt with the field of a distillery industry, in particular with methods of production of a food rectified alcohol. The method provides for digestion of the alcohol from a brew in a brew column with transition of ethyl alcohol and accompanying impurities together and with a vapor from this column in a brew distillate, purification of the brew distillate from the head and intermediate impurities including components of the fusel oil in an epuration column with feeding of hot water onto its upper plate, fractionation of the epurate in the alcohol column with separation of fractions of fusel oil, fusel alcohol and unpasteurized alcohol, distillation of fractions of the head and intermediate impurities of the ethyl alcohol in the distillation column. The faction of fusel alcohol is separated from a vapor phase of the 16-40-s plates of an alcohol column and direct to a vapor phase of a bottom of an additional column, onto the upper plate of which hot water is fed. From the condenser of the additional column they separate a concentrate of intermediate impurities. The bottom liquid of the additional column is directed together with factions from condensers of alcohol and methanol columns, as well as alcohol trappers of clear distillates onto the upper plate of the distillation column. the alcohol traps of pure distillates. Hot water is fed into the upper zone of the distillation column for hydroselection of the head impurities, propyl alcohols and other intermediate impurities, which are extracted from the condenser of this column in the form of a concentrate of the head impurities and propyl alcohols, and the bottom liquid of the distillation column is directed on a feeding plate of the epuration column. The invention allows to raise quality of alcohol.

EFFECT: the invention allows to raise quality of alcohol.

2 ex

FIELD: distillery industry; production of alcohol.

SUBSTANCE: the invention presents a method of production of a rectified alcohol and is dealt with the field of a distillery industry, in particular with methods of production of a food rectified alcohol. The method provides for digestion of the alcohol from a brew in a brew column with transition of ethyl alcohol and accompanying impurities together with a vapor from this column in a brew distillate, purification of the brew distillate from the head and intermediate impurities including components of the fusel oil in an epuration column with feeding of hot water onto its upper plate, fractionation of the epurate in the alcohol column with separation of fractions of fusel oil, fusel alcohol and unpasteurized alcohol, distillation of fractions of the head and intermediate impurities of the ethyl alcohol in the distillation column. The fusel alcohol from the alcohol column and fractions from the condensers of the alcohol column and the methanol column are fed onto the upper plate of the distillation column and also the alcohol traps of pure distillates. Hot water is fed into the upper zone of the distillation column for hydroselection of the head impurities, propyl alcohols and otherintermediate impurities, which are extracted from the condenser of this column in the form of a concentrate of the head impurities and propyl alcohols, and the bottom liquid of the distillation column is directed on a feeding plate of the epuration column. The invention allows to raise quality of alcohol.

EFFECT: the invention allows to raise quality of alcohol.

2 ex

The invention relates to techniques for the separation of multicomponent mixtures of substances on individual substances or fractions, namely, a distillation apparatus for separating bizcochada mixtures of higher aliphatic acids of number four fractions

The invention relates to the alcohol industry, in particular to methods for food rectified alcohol

FIELD: distillery industry; production of alcohol.

SUBSTANCE: the invention presents a method of production of a rectified alcohol and is dealt with the field of a distillery industry, in particular with methods of production of a food rectified alcohol. The method provides for digestion of the alcohol from a brew in a brew column with transition of ethyl alcohol and accompanying impurities together with a vapor from this column in a brew distillate, purification of the brew distillate from the head and intermediate impurities including components of the fusel oil in an epuration column with feeding of hot water onto its upper plate, fractionation of the epurate in the alcohol column with separation of fractions of fusel oil, fusel alcohol and unpasteurized alcohol, distillation of fractions of the head and intermediate impurities of the ethyl alcohol in the distillation column. The fusel alcohol from the alcohol column and fractions from the condensers of the alcohol column and the methanol column are fed onto the upper plate of the distillation column and also the alcohol traps of pure distillates. Hot water is fed into the upper zone of the distillation column for hydroselection of the head impurities, propyl alcohols and otherintermediate impurities, which are extracted from the condenser of this column in the form of a concentrate of the head impurities and propyl alcohols, and the bottom liquid of the distillation column is directed on a feeding plate of the epuration column. The invention allows to raise quality of alcohol.

EFFECT: the invention allows to raise quality of alcohol.

2 ex

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