Method of separating zeotropic mixture of butyl propionate and propionic acid

FIELD: chemistry.

SUBSTANCE: method of separating a zeotropic mixture of butyl propionate and propionic acid, components of which have relative volatility close to one, includes separating said mixture by extraction rectification using sulpholane as the parting agent, taken in ratio of 1:6-7 to the starting mixture in an extraction rectification column with efficiency of 40-50 theoretical plates, wherein the reflux ratio in the column is equal to 2-3, followed by collection of butyl propionate in the distillate and the mixture of propionic acid and supholane in the bottom of the column (1); the mixture of propionic acid and sulpholane is then fed into a column for regenerating the parting agent (2) with efficiency of 8 theoretical plates and reflux ratio equal to 0.8-1; the parting agent is removed from the bottom of the column (2) and fed into column (1). Pressure in column (1) is equal to 760 mmHg and pressure in column (2) is equal to 100 mmHg.

EFFECT: simple technique, low capital costs and high quality of the obtained products.

1 dwg, 1 tbl

 

The invention relates to the field of basic organic synthesis, namely the method of separation of zeotrope blend butylphosphonate (BP) - propionic acid (PC), the components of which have a relative volatility close to unity.

The known method of separation of this mixture extractive rectification (RAP) at a pressure 104,9 mm Hg.CT., when this mixture contains two azeotropic [Mityushkina I. A., Chelyuskin T. V., Frolkova A. K. Study of graphs α-lines in the system butylbromide - propionic acid oxide of mesityl // Theses. XIV International scientific and technical conference "high chemical technologies - 2008". Part 1. Volgograd, 2008. With 136; Chelyuskin T. V., Mityushkina I. A., Frolkova A. K. a Study of the contours relative volatility in ternary systems with bizeurope binary component // XIX Mendeleev Congress on General and applied chemistry: proc. Dokl., Volgograd, September 25-30, 2011. Volgograd: IUNL of VSTU, 2011. Vol. 1. S. 424; Chelyuskin T. V., Mityushkina I. A., Frolkova A. K., M. A. Chernysheva Separation bizeurope mixtures using additional volatile substances // Chemical technology. 2011. No. 12. S. 730-736].

The disadvantages of this method include the complexity of the technology, which is to use trekhkolesnogo complex RAP and you need double reextracting R�typicaly, that is, the presence of two columns RAP, which is connected with the necessity of compensation for the actual decrease in the selectivity of volatile separating agent (RA) due to its predominant transition to the vapour phase.

The closest technical solution of the present invention and the achieved result is a process of extractive rectification (AR) mixture butylbromide - propionic acid with dimethylsulfoxide (DMSO) at 104,9 mm Hg.PT. [T. 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; Mityushkina I. A. Division binary bizeurope mixtures using additional substances of different volatility: dis.... Cand. tech. Sciences. M: MITHT, 2011. 217 p.; Chelyuskin T. V. Theoretical foundations of distillation separation bizeurope mixtures: dis.... doctor. tech. Sciences. - M.: MITHT, 2011. 196 p.].

Best separation results are obtained under the following conditions. The efficiency of the column AR is 50 theoretical plates (T. T.), the initial mixture butylbromide-propionic acid serves 30 T. T., (counting from the top), a separating agent is dimethyl sulfoxide - 10 T. T. the Ratio of the initial mixture (F0) to the separating agent (RA) is 1:0,5. Fragmovie number is 7. The top product is butylphosphonate (9,19%) with the content of dimethyl sulfoxide (6,81%); the bottoms product of the column AR (1) - a mixture of propionic acid and dimethylsulfoxide almost equal concentrations (48,04% 51,81%) with an admixture of butylphosphonate (0,15%).

The disadvantage of the prototype is the lack of a scheme of a complete separation of the mixture butylbromide - propionic acid (considered only the column extractive distillation). DMSO forms an azeotrope with the components of the initial mixture that is not possible to distinguish the target product of a given quality in a column of AIR, and also makes impossible the separation of the initial mixture on clean components.

The technical result of the invention is to simplify the technology and reduce capital costs and improve the quality of the products.

The technical result is achieved by a method of separation of zeotrope blend butylbromide - propionic acid, the components of which have a relative volatility close to unity, including the separation of this mixture by the method of extractive distillation using as a separating agent sulfolane (SF) taken in the ratio 1:6-7 to the initial mixture in the column extractive distillation (ED) efficiency 40-50 T. T., and fregmove the number in the column is 2-3, then produce a selection of butylphosphonate in the distillate and a mixture of propionic acid sulfolane in the cube columns (1); then the mixture� PC-SF is supplied to the column regeneration of the separating agent (2) efficiency 8 T. T., the value of the reflux ratio is 0.8-1, from the cube column (2) displays a separating agent and is fed to column (1). The pressure in the column (1) is 760 mm Hg.CT., and the pressure in the column (2) is 100 mm Hg.PT. in connection with the possible decomposition of sulfolane at a temperature of 230°C. At 100 mm Hg.PT. the temperature of the bottoms product is 206.80°C-207.17°C.

The forecast of possible products of extractive rectification is based on the analysis of changes in the relative volatility of the share components in the presence of different amounts of the separating agent (RA). With the help of computational experiments was calculated vapor-liquid equilibrium in the system butylbromide - propionic acid sulfolane concentration in sections of the triangle with the concentration of SF 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 molar fraction; is the α-lines in the concentration simplex ternary systems, which showed that in the presence of SF increases the volatility of BP and sulfolane has a selectivity that is sufficient for the separation of the mixture of BP-PC extractive rectification.

Technological scheme of the process of extractive distillation for separation of binary zeotrope mixture consists of two columns (Fig.1). In a distant part of the first column AR (1) source serves a mixture of BP-PC equimolar composition in an amount of 1 KMOL/h and SF injected � 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 7. In the distillate of the first column taken almost pure butylphosphonate, and the distillation product of the binary blend of PC-SF) is sent to the next column to the regeneration of the separating agent (2), which comes in a cube of pure separating agent and is returned to the column (1). The distillate of the column (2) is an almost pure propionic acid. In columns (1) and (2) supported by various pressures, in particular in column (1) 760 mm Hg.PT. in column (2) 100 mm Hg.PT. respectively. The separation process focused on obtaining the products (butylphosphonate and propionic acid) with a purity of at least 99.5 mol%.

Conducted computer research over 70 different modes of columns separation schemes. To select the optimum mode varied the following parameters columns: efficiency (number of theoretical plates); the ratio of the quantities of food and separating agent; fregmove the number and grades of the filing of the original mixture and the RA.

Examples of modes of operation of the scheme of separation of zeotrope blend butylbromide-propionic acid, which achieved the required quality of the products that are listed in the table.

Thus, we propose a process flow diagram of a complete separation of zeotrope blend butylbromide - propio�OIC acid, components which have a relative volatility close to unity, using magelonidae separating agent is sulfolane. The proposed method allows to obtain the desired products (PD, PC) of a given quality - 99.5 mol%.

Modes of operation of the circuit split bizeurope mixture butylbromide - propionic acid;

No. exampleThe operating parameters of the column (R-fregmove number, F0/PA-power ratio and the separating agent,
N(1)N(2)- (Qty T. T. in columns 1, 2)
The original mixtureA separating agentGrocery streams
Number, KMOL/hComposition, mol %Number, KMOL/hComposition, mol%.BPPC
BPPCNumber, KMOL/hComposition, mol%.Number, KMOL/hComposition, mol%.
1N1=501505061000,599,800,5by 99.79
N2=8
R1=2
R2=0,8
F0/PA=1/6
2N1=501505061000,599,810,5by 99.79
N2=8
R1=3
R2=0,8
F0/PA=1/6
3N1=5015050 71000,599,900,599.91 per
N2=8
R1=2
R2=0,8
F0/PA=1/7
4N1=451505061000,599,520,599,55
N2=8
R1=2
R2=0,8
F0/PA=1/6
5N1=451505061000,599,570,5 99,58
N2=8
R1=3
R2=0,8
F0/PA=1/6
6N1=451505071000,599,690,599,71
N2=8
R1=2
R2=0,8
F0/PA=1/7
7N1=401505061000,598,550,598,57
N2=8
R1=2
R2=0,8
F0/PA=1/7
8N1=401505071000,5RUB 99.560,599,58
N2=8
R1=3
R2=0,8
F0/PA=1/7

Method of separation of zeotrope blend butylphosphonate (BP) - propionic acid (PC), the components of which have a relative volatility close to unity, including the separation of this mixture by the method of extractive distillation using as a separating agent sulfolane (SF) taken in the ratio 1:6-7 to the initial mixture in the column extractive distillation efficiency 40-50 theoretical plates (T. T.), and fregmove the number in the column is 2-3, then produce a selection of butylphosphonate in the distillate and a mixture of propionic acid sulfolane in the cube columns (1); the mixture is then PC - SF is supplied to the column regeneration of the separating agent (2) efficiency 8 T. T., the value of reflux ratio amounted to�ing 0.8-1, from the cube column (2) displays a separating agent and is fed to column (1), the pressure in the column (1) is 760 mm Hg.CT., and the pressure in the column (2) is 100 mm Hg.PT.



 

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