Method of system separation: benzol-perfluorobenzol-tertiary amyl alcohol

FIELD: chemistry.

SUBSTANCE: method includes supply of initial mixture and dimethylsulfoxide (DMSO) as separating agent, taken in ratio 7-7.5:1 to initial mixture, into extraction rectification column (1) efficiency 50 t.t., initial mixture being supplied on 30 t.t., separating agent on 10 t.t. of column (plate numeration from top of column), phlegm number in column constitutes 1.5-2, taking of benzol in distillate and mixture benzol-perfluorobenzol (PFB) - tertiary amyl alcohol (TAA)-DMSO from column (1) cube , supply of mixture PFB-TA-DMSO on 25 t.t. of column of separating agent regeneration (2) with efficiency 50 t.t., phlegm number in column being 1-3, removal separating agent from column cube and its supply to column (1), supply of column (2) distillate, representing aseotropic mixture PFB-TAA, for separation into complex of two columns (3) and (4) with efficiency 35 t.t., with removal from column cubes of TAA and PFB, respectively, aesotropic mixture being supplied on 18 t.t. of column (3), phlegm numbers of columns (3) and (4) being equal 0.5-1.5 and 1-2 respectively, re-cycle of aseotrope PFB-TAA, which is separated in distillate of column (4) into column(3) feeding, ratio of re-cycle of column (4) and feeding of column (3) being (1-1.1):0.66, pressure in columns (1)-(3) is 300 mm of mercury, pressure in column (4) - 760 mm of mercury.

EFFECT: simplification of technology, increase of ecological compatibility of process and quality of obtained products.

1 tbl, 1 dwg, 1 ex

 

The invention relates to the field of organic synthesis, and particularly to a method of separation bizeurope mixture of benzene-performanta-tertiary amyl alcohol.

Benzene is included in the composition of gasoline, is widely used in industry, is the raw material for the production of drugs, various plastics, synthetic rubber and dyes. Performanta used in laboratory practice for synthesis of polyfluoroaromatic compounds and as a solvent.

There is a method of separating such a mixture of the carboxylic acid fraction With5-C13and butyl esters. [Smokes. Higher fatty alcohols. M.: Chemistry, 1970]

In the process of obtaining higher fatty alcohols With7-C9by catalytic hydrogenation of fatty acids and their esters the first step is the esterification of the acids of the C5-C13. Since the esterification reaction is reversible, despite the continuous removal of water from the reaction mixture, it is not possible to obtain esters without impurity acids (butyl esters contain from 2 to 5% of unreacted acids). Therefore, the crude ester is neutralized with 25%-rastvorom alkali to remove acids, unreacted. From the neutralizer selected three layers: ether containing pure butyl esters, alkaline and intermediate (emulsion). Emulsion layer, which which contains esters and unreacted carboxylic acid, collect in a container, and again sent to the Converter. The alkaline solution of sodium salts of fatty acids (Soaps) are separated from the esters by settling and treated with sulfuric acid. Thus regenerate the free acid, which after washing with water is separated from the sodium sulfate and again return to production. Esters are washed in the neutralizer with water and dried in vacuum. When washing produce large quantities of waste water, so washing is sometimes replaced by distillation.

The disadvantages of this method include the complexity of technology, the formation of large quantities of sewage, polluting the environment, and the need to use corrosion resistant materials, since the process takes place in the presence of sulphuric acid.

Share the mixture described above, and the mixture described in this invention contain binary bizeurope component.

The technical result of the proposed method is to simplify the technology, improving the environmental friendliness of the process and quality of the products.

This technical result is achieved by using for the separation of a three component system with binary bizeurope component method of extractive distillation.

As the source of the selected triple basetsana system: benzene (B)-performanta (PFB)-Tretij the first amyl alcohol (TAS). As a separating agent (RA) selected polar solvent is dimethyl sulfoxide (DMSO), often used in the processes of extraction separation.

The forecast of the possible products of extractive distillation was carried out on the basis of the analysis of changes in the relative volatility in the presence of different amounts of RA in the respective phase diagrams. Using computational experiment was studied phase behavior of a mixture of B-PFB-TAS in the presence of DMSO and its separation by extractive distillation.

The analysis was performed on the phase behavior of the Quaternary system in the sections of the tetrahedron with a constant concentration of DMSO (0.2, 0.4, 0.6 and 0.8 molar fractions). For each section of the received data arrays vapor-liquid equilibrium (AHC) and using the relative shares of the original components in the liquid phase (X1, X2, X3built appropriate charts the progress of a single α-lines. According to the AHC in the triple components built single α-lines on the faces of the tetrahedron. In the end, there was obtained a General picture of the progress α-surfaces in the concentration simplex four-part system, which allowed to evaluate the possibility of separating a mixture of B-PFB-TAS extractive rectification.

In this work, the developed circuit split triple baserape mixture, the cat heaven consists of 4 columns (Technological scheme of the process of extractive distillation). First column - ER (1), in a distant part of which serves original mix B-PFB-TAS equimolar composition in an amount of 1 KMOL/h, and DMSO injected into the upper section of the column. The variation value of the first recycling (number DMSO) provides the necessary selectivity separating agent for the implementation of the extractive effect. The ratio of the quantities RA and initial mixture in column (1) was changed from 1 to 10. In distillate first column select pure benzene, and a cube is a three-component mixture PFB-TAS-DMSO, which goes in the next column regeneration separating agent (2), in the cube which comes out clean separating agent and sent back to the column (1). The distillate of the column (2) is an azeotropic mixture PFB-TAS. It is directed to the separation of the complex of the two columns (3,4), working under different pressures. Cubes columns out of pure components (TAS and PPB respectively), and the distillates - azeotrope PFB-TAS. In the diagram there are two recycling: in the first column ER returns a separating agent (DMSO), in the second azeotrope recycle PFB-TAS, which is highlighted in distillate column (4). The pressure in the columns (1)-(3) - 300 mm Hg, in column (4) is 760 mm Hg separation Process is focused on getting the products (benzene, performante and tertiary amyl alcohol) with a purity of 99.5 mol.%.

Held computer research more than 50 different modes of columns separation schemes. To select the optimal mode varied the following parameters of the pillars: the height (number of theoretical plates), size recyclo, reflux number.

The optimal ratio of the recycle column (4) and supply columns (3) is (1-1,1):0,66, which corresponds to the desired target products TAS and PFB.

The required quality of products is achieved when the following parameters columns: column (1) efficiency 50 TT, the filing of the original mixture for 30 TT separating agent 10 TT (the numbering of the plates from the top of the column), reflux the number of 1.5-2.0; a ratio of the amounts of the separating agent and the initial mixture (7-7,5):1; column (2) efficiency 50 CT, power supply 25 TT, reflux number of 1,0-3,0; columns (3), (4) efficiency 35 CT, power supply 18 TT, reflux ratio equal to 0.5-1.5 and 1.0-2.0, respectively.

Thus, the used method allows to obtain the target products (B, PFB, TAS) given quality - of 99.5%, to simplify the existing technology and improve ekologichnost process due to the absence of sewage.

td align="center" morerows="4"> 100
The material balance of the process of separating a mixture of benzene - performanta - tertiary amyl alcohol in the presence of dimethylsulfoxide.
Table
# example Parameters columns (R - reflux number PA/F0- the ratio of the separating agent and nutrition)The initial mixtureA separating agentProduct streams
Composition, mol.%BPFBTAS
Qty, KMOL/hBPFBTASQty, KMOL/hComposition, mol.%Qty, KMOL/hComposition, mol.%Qty, KMOL/hComposition, mol.%Qty, KMOL/hComposition, mol.%
1R1=1.5134333371000,3499,80,331000,3399,8
R2=1.0
R3=0.5
R4=1.0
PA/F0=7:1
2R1=2134333370,3499,80,3399,80,3399,9
R2=1.0
R3=0.5
R4=1.0
PA/F0=7:1
3R1=2134333371000,3499,80,3399,80,33100
R2=2
R3=0.5
R4=1.0
PA/F0=7:1

The method of separating a mixture of benzene-performanta (PFB)-tertiary amyl alcohol (TAS), including the filing of the original mixture and dimethyl sulfoxide (DMSO) as a separating agent, taken in the ratio of 7-7,5:1 to the original mixture to extractive distillation column (1) efficiency 50 TT, and the initial mixture serves 30 TT separating agent 10 TT columns (the numbering of the plates from the top of the column), and reflux the number in the column is 1.5-2, the selection of benzene in distillate and mixtures PFB-TAS-DMSO from the cube columns (1)feeding a mixture PFB-TAS-DMSO at 25 TTH column regeneration separating Agay is that (2) efficiency 50 TT, and reflux the number in the column is 1-3, the output from the cube columns separating agent and filing it in column (1), the filing of distillate columns (2), which is an azeotropic mixture PFB-TAS, separation of the complex of the two columns (3) and (4) efficiency 35 TT with the removal of the cubes columns TAS and PPB, respectively, and the azeotropic mixture is served on 18 TT columns (3)and reflux ratio of columns (3) and (4) 0.5-1.5 and 1-2, respectively, recycling azeotrope PFB-TAS that is distillate column (4) in the power of the column (3), and the ratio of the recycle column (4) and supply columns (3) is (1-1,1):0,66, the pressure in the columns (1)-(3) is 300 mm Hg, and the pressure in column (4) is 760 mm Hg



 

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FIELD: chemistry.

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11 cl, 1 tbl, 1dwg, 1ex

FIELD: chemistry.

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8 cl, 3 tbl, 4 ex

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2 tbl, 10 ex

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12 cl, 1 dwg, 3 tbl, 6 ex

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15 cl, 1 dwg, 1 tbl, 2 ex

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