The method of separating a mixture of acetochlor azeotropic composition of extractive rectification

 

The invention relates to chemical technology. The method is realized by means of extractive distillation using as the extractive agent in dimethylformamide complex column with lateral section. The effectiveness of the main column 34 so so, the efficiency of the side sections 10 so so Reflux ratio in the main column and sidebar sections are (0,41-0,42) and (2,8-5,8), respectively. Selected as the main column distillate commodity acetone, in a cube - dimethylformamide, and in the distillate side of the section - chloroform. The technical result - the reduction of energy consumption, improvement of the quality of the target product. table 1.

The invention relates to the field of chemical technology, in particular to a method of distillation separation of the azeotropic mixture of acetone-chloroform. The problem of separation of the mixture occurs when you create a block regeneration of solvents used in the production of thermo stabilizer Stabilin-9.

Recently, for the separation of azeotropic mixtures more practical application is a method of extractive distillation, which often turns out to be energetically more favorable than the separation in columns under different pressures. Of the cation as separating agents of water and dimethylformamide (DM F).

In the patent (patent Germany 1083823, CL 07 b, 1960) for separating a mixture of acetone-chloroform azeotrope composition as a separating agent is proposed to use the water. Technological scheme of the process includes two columns. In the first column efficiency 30 plates serves the initial mixture containing 25 wt. % acetone and 75 wt.% the chloroform. Water is fed to the upper level of the column. Reflux the number is 1. As distillate selected chloroform mixed with acetone 0.03 wt.%. CBM product composed of a mixture of acetone and water, rectificatum in the second column.

The disadvantages of this process should include the complexity of the separation of the bottom product of the first column, because a mixture of acetone-water at a pressure of 760 mm RT.article characterized by the presence of tangential azeotrope, which requires to achieve the required quality of the acetone column efficiency or carry out the process under reduced pressure. In addition, when using water as the extractive agent in the distillate of the first column may exfoliating product that to obtain chloroform high quality will require installation of Florentine vessel and host additional purification.

The closest in technical SUWANEE other extractive agent of dimethylformamide (A. C. 1366173, CL 01 D 3/16, C 07 C 19/04, 49/08, 1988 - T., Pavlenko, A. K. Frolova, L. A. Tart, C. M. Kareeva and B. C. Timofeev. The method of separating a mixture of acetone-chloroform azeotrope composition). Technological scheme consists of two columns - column extractive distillation (column 1) and column regeneration extractive agent (column 2). The original azeotropic mixture composition is fed to the middle of the column 1, the extractive agent is on the upper level. As the distillate of the extractive column select acetone containing 1.1 wt.% chloroform and in the form of a bottom liquid - mixture of chloroform and DMF, which is divided in the second column with reflux, equal to 1.3-1.5. The top product is an almost pure chloroform. CBM thread - DMF mixed with chloroform not more than 0.1 wt.% - return on irrigation in the first column. The efficiency of the extractive distillation column 15 so-so, and column regeneration extractive agent 12 so so

The disadvantage of the prototype is the process in two columns, which requires the installation of pumps, piping and intermediate tanks for pumping a bottom liquid of the first column to the second and additional energy consumption for evaporation of the fluid in kobaian, requirements for the technical acetone, whereby the impurities should not exceed 0.5 wt.% The technical essence of the present invention is the reduction of energy consumption for the separation of a mixture of acetone-chloroform and receive acetone, corresponding to the technical product.

This goal is achieved by the process of extractive distillation in a single complex string with the side section. The effectiveness of the main column 34 so so, the efficiency of the side sections 10 so so Reflux number in the main column 0,41-0,42; in the side sections of 2.8 to 5.8. The original mixture of acetone-chloroform azeotrope composition serves at boiling point on the 11-th plate of the main column, the extractive agent at a temperature of 20oWith - in 5 a plate. The mass ratio of the initial mixture and of dimethylformamide is 1: (2.0 to 2.5). The steam flow is taken into a side section with 23 plates of the main column, the flow of fluid from the side of the section return on the same plate. As distillate main column select acetone with a total content of chloroform and DMF 0.5 wt.% CBM product - DMF mixed with chloroform 0.1 wt. % - return on irrigation in the 5-th plate of the main column. Chloroform mixed with Ni separation of 100 kg/hour of a mixture of acetone-chloroform azeotrope composition, calculated by computational experiment, when the ratio of the initial mixture : DMF=2,5 make 0,1476 GJ/hour, and the total heat load in the boilers schema-prototype - 0,2063 GJ/hour.

Thus, the organization of the process in the same column with side panel allows to reduce energy costs by 28.5% compared with the scheme of the prototype and get acetone higher quality (of 99.5 wt.% unlike the 98.9 wt.% for the schema of the prototype) with the same ratio of the initial mixture:DMF.

Claims

The method of separating a mixture of acetochlor azeotropic composition of extractive distillation using as the extractive agent dimethylformamide, characterized in that the process is carried out in a complex column with lateral section, and the effectiveness of the main column 34 so so, the efficiency of the side sections 10 so-so, and the reflux ratio in the main column and sidebar sections are (0,41-0,42) and (2,8-5,8), respectively, with the selection in the main column distillate commodity acetone, in a cube - dimethylformamide, which returns to irrigation in the upper part of the main column, and in the distillate side sections of chloroform.

 

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