Method of separating biazetropic mixture butylpropionate-propionic acid

FIELD: chemistry.

SUBSTANCE: to separate a biazetropic mixture butylpropionate-propionic acid used is a method of extractive rectification with application as a separating agent of sulpholane (SF), taken in ratio 1:5-6 to an initial mixture in a column of extraction rectification with efficiency 35-50 t.t., with reflux ratio in the column being 1-3. Withdrawal of butylpropionate in distillate and the mixture propionic acid-sulpholane in the column bottom is carried out. After that, the mixture PC-SF is supplied to the column of the separating agent regeneration with efficiency 8 t.t., value of reflux ratio is 0.5-1.0. The separating agent is withdrawn from the column bottom and supplied into the column. Pressure in the columns constitutes 100 mm Hg. The method makes it possible to obtain the target products (BP, PA) of a specified quality - 99.5 mol%.

EFFECT: simplification of technology and reduction of capital expenditure, increased quality of obtained products.

1 dwg, 1 tbl

 

The invention relates to the field of organic synthesis, namely the method of separation bizeurope mixture butylphosphonate (BP)-propionic acid (PC).

The known method of separation of this mixture extractive rectification (RAP) at a pressure of 104,9 mm Hg [Matushkina I.A., Chelyuskin T.V., Frolkova A.K. Study charts the α-lines in the system butylbromide - propionic acid oxide of mesityl // Abstr. XIV International scientific-technical conference "high chemical technologies - 2008". Part 1. Volgograd, 2008. S. 136; Chelyuskin T.V., Matushkina I.A., Frolkova A.K. study of the contour relative volatility in three-component systems with bizeurope binary component // of the XIX Mendeleev Congress on General and applied chemistry: abstracts. Dokl., Volgograd, 25-30 September 2011. Volgograd: INL VSTU, 2011. Vol. 1. S;

Chelyuskin T.V., Matushkina I.A., Frolkova A.K., Chernysheva M.A. Division bizeurope mixtures with the use of more volatile substances. // Chemical technology. 2011. No. 12. S-736].

The disadvantages of this method include the complexity of technology, which is to use trehkolonnom complex RAP and the need of dual extractive rectification, i.e. the presence of two columns RAP, which is connected with the necessity of compensating the actual reduction is possible selectivity volatile separating agent (RA) due to its predominant transition in the vapor phase.

The closest technical solution of the present invention and the achieved result is a process of extractive distillation (ER) mixture butylbromide-propionic acid with dimethyl sulfoxide (DMSO) at 104,9 mm Hg[I.e Chelyuskina, I.Mityushkina, A.Frolkova. Estimation of possibility of industrial mixture separation by extractive rectification // Proceedings 35th International Conference of Slovak Society of Chemical Engineering. Tatranske Matliare. Slovakia, May 26-30, 2008. P.174; Matushkina I.A. Division binary bizeurope mixtures with the use of additional substances of different volatility: dis....Kida. technology. Sciences. M: MITHT, 2011. 217; Chelyuskin T.V. Theoretical foundations distillation separation bizeurope mixtures: dis.... Prof. technology. Sciences. - M.: MITHT, 2011. 196 S.].

The best separation results obtained under the following conditions. The efficiency of the column ER 50 theoretical plates (TT), original mix butylbromide-propionic acid serves 30 CT, (counting from the top), a separating agent dimethyl sulfoxide at 10 TT the Ratio of the initial mixture (F0) to the separating agent (RA) is 1:0.5 in. Reflux the number is 7. The top product is butylphosphonate (93,19%) containing dimethyl sulfoxide (for 6.81%); CBM product columns ER (1) - a mixture of propionic acid and dimethyl sulfoxide almost equal concentrations (48,04% 51,81%) mixed with butylphosphonate (0,15%).

The disadvantage of p is ototype is the absence of a schema complete separation bizeurope mixture butylbromide-propionic acid (considered only column extractive distillation). DMSO forms azeotrope with components of the original mixture, which is not allowed to select the target product of a given quality in the column ER and made it impossible to split the original mixture into pure components.

The technical result of the present invention is to simplify the technology and capital cost reduction, and improving the quality of the products.

The technical result is achieved by the method of separation bizeurope mixture butylbromide-propionic acid, including extractive distillation using as the separating agent sulfolane (SF), taken in the ratio 1:5-6 to the original mixture in the column ER efficiency 35-50 TT, and reflux the number in the column is 1-3, are selected butylphosphonate in the distillate and the mixture propionic acid-sulfolan columns in the cube (1); then the mixture of PC-SF is fed into the column regeneration separating agent (2) efficiency 8 TT, the value of the reflux ratio is 0.5-1, from the cube column (2) displays a separating agent and served in column (1). The pressure in the columns (1)-(2) is 100 mm Hg

The forecast of the possible products of extractive distillation was carried out on the basis of the analysis of changes in relative volatility of shared components in the presence of different amounts of RA. Using computational experiment Belorussian vapor-liquid equilibrium in the system PSU-PC-SF in sections of the concentration triangle with a concentration of sulfolane 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 molar fractions; built the course of the α-lines in the concentration simplex three-component system, which showed that in the presence of SF increases volatility BP and sulfolan is selective enough to separate the mixture of BP-PC extractive rectification.

Technological scheme of the process of extractive distillation separation of a binary bizeurope mixture consists of two columns (figure 1). In a distant part of the first column ER (1) submit original mix PSU-PC equimolar composition in an amount of 1 KMOL/h, and SF is introduced into the upper section of the column. The ratio of the number of RA and the initial mixture in the column (1) is changed from 1 to 6. In the distillate of the first column selected is almost pure butylphosphonate and CBM product (binary mixture of PC-SF) sent in the following column regeneration separating agent (2), in the cube which comes out clean separating agent and returned back to the column (1). The distillate of the column (2) represents almost pure propionic acid. In columns (1) and (2) is supported by the pressure of 100 mm Hg separation Process is focused on getting products (butylphosphonate and propionic acid) with a purity of at least 99.5 mol.%.

Conducted computer analysis of more than 70 different modes of columns separation schemes. To select the optimal mode warier who were following parameters pillars: efficiency (number of theoretical plates), the ratio of the quantities of food and separating agent, reflux the number and levels of the filing of the original mixture and RA.

Examples of modes of separation schemes bizeurope mixture BP-PC, which achieved the desired quality of the products, are given in table 1.

Thus, we propose a method that includes the principal technological scheme of the complete separation bizeurope mixture butylbromide-propionic acid using magelonidae separating agent is sulfolane. The proposed method allows to obtain the target products (BP, PK) given quality of 99.5 mol.%.

Table 1
Modes of separation schemes bizeurope mixture butylbromide-propionic acid
# exampleThe operating parameters of the column (R - reflux number, Fo/PA - ratio power supply and a separating agent, N(1)N(2)- (Qty TT in connah 1, 2)The initial mixtureA separating agentProduct streams
Qty, KMOL/hWith the Tav,mol.% Qty, KMOL/hComposition, mol.%BPPC
BPPCQty, KMOL/hComposition, mol.%Qty, KMOL/hComposition, mol.%
1N1=501505051000,599,900,599,86
N2=8
R1=1
R2=0,5
F0/PA=1/5
2N1=501505051000,5 at 99.950,599.91 per
N2=8
R1=2
R2=0,5
F0/PA=1/5
3N1=501505061000,599,990,599,88
N2=8
R1=1
R2=0,5
F0/PA=1/6
4N1=401505051000,599,540,599,59
N2=8
R1=1
R2=0,5
F0/PA=1/5
5N1=401505051000,599,740,599,70
N2=8
R1=2
R2=0,5
F0/PA=1/5

6N1=401505061000,599.89 per0,599,79
N2=8
R1=1
R2=0,5
F0/PA=1/6
7N1=351505051000,599,530,599,51
N2=8
R1=1
R2=0,5
F0/PA=1/5
8N1=351505051000,599.89 per0,599,86
N2=8
R1=2
R2=0,5
F0/PA=1/5
9N1=3515050 51000,599,930,599,84
N2=8
R1=1
R2=0,5
F0/PA=1/6

The method of separation bizeurope mixture butylphosphonate (BP) - propionic acid (PC), including extractive distillation, characterized in that the separating agent used sulfolan (SF), taken in the ratio 1:5-6 to the original mixture in the column (1) extractive distillation efficiency 35-50 theoretical plates (TT), with the value of the reflux ratio in the column - 1-3, and the selection of butylphosphonate produce a distillate and a mixture of propionic acid-sulfolan in Cuba columns (1), then a mixture of PC-SF fed to the column regeneration separating agent (2) efficiency 8 TT, with a value of reflux ratio of 0.5 - 1, from the cube column (2) derive a separating agent and served in column (1), the pressure in columns (1)-(2) is 100 mm Hg



 

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