Method of extraction of butanol, butyl acetate and water from a mixture of

 

(57) Abstract:

Usage: in chemical technology. Essence: allocation of butanol, butyl acetate and water from the mixture. Pre-cleanse is a partial mixture of impurities, such as biological, in a rotary film evaporator with a bit of selection in the distillate from 0.90 to 0.92. Distillates rotary film evaporators rasclaat in the water separators and organic layers. Water layers return on irrigation rotary film evaporators, and the organic layers emit a mixture of butanol and butyl acetate by azeotropic distillation in Cuba distillation column with reflux 0.3 - 1.0 and share selection in the distillate of 0.5 - 0.7. The distillate is a triple mixture of water, butanol and butyl acetate to the azeotrope, rasclaat in the separator on the water and organic layers. The aqueous layer was returned to the irrigation of a rotary film evaporator and the organic layer is recycled to distillation column for separation of a mixture of butanol and butyl acetate. Removing the butyl acetate is carried out by azeotropic distillation of the mixture of butanol and butyl acetate at reflux the number from 1.0 to 2.0 and share selection in the distillate from 0.6 to 0.7 with getting in distillate mixture of butanol and butyl acetate azeotrope including 4,0 - 5.0 and share selection in distillate of 0.75 to 0.8. In distillate columns heterotetramer rectification receive a mixture of water, butanol and butyl acetate. The distillate is rasclaat in the separator water layer, which return for the allocation of butanol, and the organic layer, which is mixed with an organic layers rotary film evaporators for separation of a mixture of butanol and butyl acetate. 1 Il.

The invention relates to chemical technology, and in particular to methods of separation hardly separated commercial mixtures containing butanol, butyl acetate and impurities, e.g., biological, such as antibiotic products of inactivation, pigments, and can be used in chemical, pharmaceutical, paint and other industries.

In the production of potassium salt of benzylpenicillin as solvents used butanol, butyl acetate and water. In the process there is a mixing of solvents and pollution of their biological impurities. The result is the formation of two streams of waste solvents, one of which contains mainly butanol and contaminated with butyl acetate, water, and dissolved impurities. The second stream mainly consists of butyl acetate is canola and butyl acetate without regeneration.

There is a method of regeneration of butanol in the production of penicillin, based on a combination of semi-continuous distillation with continuous heterotetramer rectification. In the first stage of the method of the regenerated cleaning solution from the non-volatile and high-boiling impurities are separated in a distillation installation, representing the cube is equipped with an external heater. In the second stage, the organic layer of the distillate formed in the decanter in the separation of the condensed vapors are subjected to dehydration in nepreryvnolitoy distant distillation column. Dehydrated butanol is removed from the column in the form of the cubic product [1]

The disadvantage of this method is the accumulation in the target butanol butyl acetate, removal of which it is proposed to apply periodic saponification with caustic soda boiling, which, in turn, leads to the formation of large amounts of wastewater and loss for the expensive production of butyl acetate.

The closest in technical essence and the achieved result to the invention is a method of distillation of butanol, butyl acetate and water, including the allocation of butanol and butyl acetate in the cubes rectify the e and organic layers in cages. At the same time as recycle streams use the organic layers of separators, and water butanol strictly defined concentration. For implementing the method serves the initial mixture containing butanol, butyl acetate and water, the first distillation column, from the cube which are selected butyl acetate. To translate the composition of the initial mixture of the second column in the area of compositions that are favorable for separation of butanol from the cube of the second column, for distillate the first column add additional recycle stream of water and butanol such that the difference of the concentration of butanol in the distillates of the first and second columns was positive. The selection of butanol is carried out at reflux 16. The allocation of water is performed by the method of azeotropic distillation in the third column. Distillates of the second and third distillation columns comprising water, butanol and butyl acetate, subjected to delamination in two separators, the aqueous layers are combined into one stream and fed to the rectification in the third column, and the organic layers are returned to the first distillation column. From the cube to the third pillar drains [2]

However, adding to distillate first distillation column additional flow vodnala return butanol and butyl acetate production and protect the environment from pollution, and increases the complexity of managing the separation process. In addition, the disadvantage of this method is the formation of scale on the plates of distillation columns, leading to premature columns of the system and, therefore, exclude the application of the method in the pharmaceutical industry, which is the result of a lack projectification partial purification of a mixture of impurities, such as biological.

The invention consists in that in the known method of separation of butanol, butyl acetate and water from the mixture, including the allocation of butanol and butyl acetate in cubes of distillation columns by azeotropic distillation and separation of distillate products of rectification on the water and organic layers in the separators, the recycle stream is used layers of separators, pre-cleaned a partial mixture of impurities in a rotary film evaporator with a bit of selection in the distillate is between 0.90 and 0.92, distillates rotary film evaporators rasclaat in the water separators and organic layers, return water layers on irrigation rotary film evaporators, and organic layers emit a mixture of butanol and butyl acetate is the distillate from 0.5 to 0.7, obtained when the distillate is rasclaat in the separator on the water and organic layers, return water layer on irrigation rotary film evaporator, and the organic layer recycle for separation of a mixture of butanol and butyl acetate, butyl acetate extraction is carried out by azeotropic distillation of the mixture of butanol and butyl acetate at reflux the number from 1.0 to 2.0 and share selection in the distillate from 0.6 to 0.7 with getting in distillate mixture of butanol and butyl acetate azeotrope composition, which produce butanol by heterotetrameric distillation with water at reflux the number from 4.0 to 5.0 and share selection in the distillate from 0.75 to 0.8, the distillate of the column heterostrophus rectificate and consisting of a mixture of water, butanol and butyl acetate, rasclaat in the separator water layer, which return for the allocation of butanol, and the organic layer, which is mixed with an organic layers rotary film evaporators for separation of a mixture of butanol and butyl acetate.

The technical result is the return of butanol and butyl acetate in the production and reduction of emissions into the environment, reducing the complexity of the process control division, improving the performance of rectifica the th environment is achieved by increasing the degree of separation of butanol and butyl acetate, namely, the selection of butanol and butyl acetate, purity 99,0% of the mixture.

Reducing the complexity of the management process of separation is achieved due to use as recycle streams only layers of separators that stabilizes the process. This eliminates the preparation and input of additional water flow butanol.

Improving the performance of distillation columns is provided by eliminating scale formation on the plates of distillation columns, i.e., the introduction of pre-treatment separable mixtures of impurities, such as biological, rotary film evaporators.

The invention is illustrated by a drawing, which shows a selection scheme butanol, butyl acetate and water from the mixture.

Method of extraction of butanol, butyl acetate and water from a mixture as follows. A mixture of F1and F2waste butanol and butyl acetate containing particles, such as biological, pre-cleaned of these impurities in a rotary film evaporators 1 and 2. Impurities contained in the mixtures F1and F2waste butanol and butyl acetate, remove from water W1, W2cube p is 2 rasclaat in the separators 3 and 4 in aqueous and organic layers. Water layers V3and V4Wasserman for irrigation rotary film evaporators 1 and 2, and the organic layers O3and O4sent for rectification in the column 5. Cleansing in a rotary film evaporators spend with the share selection in the distillate from 0.90 to 0.92, which allows you to bring butanol and butyl acetate in the composition of the distillates of D1and D2. When the proportion of selection in the distillate is in excess of 0.92, difficult abstraction of the cubic product by increasing its viscosity. When the proportion of selection in the distillate is less of 0.90, there is a contamination of the cubic product butanol and butyl acetate.

Organic layers O3and O4distillate separators 3 and 4 emit binary fraction is a mixture of butanol and butyl acetate W5by azeotropic distillation in Cuba distillation column 5. Received while the distillate D5distillation column 5, a ternary mixture of water, butanol and butyl acetate, close to the azeotrope composition, rasclaat in the separator 6 in of water V6and organic ABOUT6the layers. The aqueous layer V6served with a mixture of waste butanol and butyl acetate F1for irrigation of a rotary film evaporator 1. The organic layer O6recircu the butanol and butyl acetate in a distillation column 5 is optimally carried out at reflux the number R of from 0.3 to 1.0 and share selection in the distillate from 0.5 to 0.7. The decline in the share selection in the distillate is below 0.5 and increasing reflux ratio than 1.0 leads to contamination of the cubic product W5water. The increase in the proportion of selection in the distillate is higher than 0.7 and lower reflux ratio of less than 0.3 leads to unstable operation of the separator 6.

A mixture of butanol and butyl acetate W5sent to distillation column 7 to highlight butyl acetate W7by azeotropic distillation. In distillate D7column 7 gives a blend of butanol and butyl acetate azeotrope composition.

The allocation of butyl acetate in a distillation column 7 is optimally carried out at reflux the number R of 1.0 to 2.0 and share selection in the distillate from 0.6 to 0.7. When reflux numbers less than 1.0 and share selection in the distillate is less than 0,6 quality butyl acetate due to its dilution butanol. Increasing the reflux ratio above 2.0 and share selection in the distillate is higher than 0.7 leads to a decrease in the quantity of drained butyl acetate W7thereby unnecessarily increasing the load of the rectifying column 8.

Of distillate D7the rectifying column 7, consisting of a mixture of butanol and butyl acetate azeotrope composition, produce butanol W8in a distillation column 8 put the water, butanol and butyl acetate. This distillate D8rasclaat in the separator 9 to the water layer Vgand the organic layer O9. The aqueous layer V9return to the distillation column 8 for irrigation. The organic layer O9mixed with organic layers O3and O4rotary film evaporators 1 and 2 for separation of a mixture of butanol and butyl acetate in a distillation column 5.

The selection of butanol in a distillation column 8 is optimally carried out at reflux the number R of from 4.0 to 5.0 and share selection in the distillate from 0.75 to 0.8. When reflux numbers less than 4.0 and share selection in the distillate is less than 0,75 contaminate butanol-butyl acetate. Increasing the reflux ratio above 5.0 and share selection in the distillate is more than 0.8 decreases the yield of butanol and increases the load on the separator 9, which leads to unnecessary increase of the recycle stream, returning the organic layer O9distillate in a distillation column 5.

The use of the invention in comparison with known provides a selection of butanol and butyl acetate, purity 99,0% of a mixture of waste solvents that will allow you to return them in production and reduce environmental emissions. In addition ETag columns.

P R I m e R 1 (optimal values). The flow of exhaust butyl acetate, containing 62 wt. butyl acetate, 11 mol. butanol and 27 mol. water and the flow of exhaust butanol containing 8 mol. butyl acetate, 37 mol. butanol and 55 mol. water, cleaned in a rotary film evaporator with a bit of selection in the distillate of 0.91, distillates rotary film evaporators rasclaat in the water separators and organic layers, return water layers on irrigation rotary film evaporators, and the organic layers emit a mixture of butanol and butyl acetate by azeotropic distillation in Cuba distillation column efficiency to 15 tons, tons, operates at atmospheric pressure and reflux the number 0.8 and share selection in the distillate of 0.6. The water content in the bottom product of the column with 0.5 mol. Obtained when the distillate is rasclaat in the separator on the water and organic layers, return water layer on irrigation rotary film evaporator, and the organic layer recycle for separation of a mixture of butanol and butyl acetate. Removing the butyl acetate is carried out by azeotropic distillation of the mixture of butanol and butyl acetate in a distillation column efficiency 10 t t operating at atmospheric pressure with flegmatisch, of which produce butanol by heterotetrameric distillation with water in a distillation column efficiency 9 so t at reflux the number 4,5 and share selection in the distillate is 0,76. The distillate of the column heterotetramer rectification, similar in composition to the composition of the ternary azeotrope, rasclaat in the separator water layer, which return for the allocation of butanol and the organic layer, which is mixed with an organic layers rotary film evaporators for separation of a mixture of butanol and butyl acetate. As the distillation products are selected butanol content of 99.7 mol. and butyl acetate content of 99.2 mol. meets the requirements of GOST.

P R I m m e R 2 (upper limit of separation options). Spent solvents of the composition given in example 1 is subjected to rectification in example 1, but at reflux to column selection of a mixture of butanol and butyl acetate = 1, and the proportion of selection in the distillate of 0.5. With these parameters, the water content in the bottom product of 0.7 mol. The allocation of butyl acetate is carried out at reflux including 2.0 and share selection in the distillate of 0.6. As the cubic product selected butyl acetate content of 99.2 mol. The selection of butanol is carried out at reflux including 5.0 and share selection in CLASS="ptx2">

P R I m e R 3 (the lower boundary of the separation options). Spent solvents of the composition given in example 1 is subjected to rectification in example 1, but at reflux to column selection of a mixture of butanol and butyl acetate, 0.3, and share selection in the distillate of 0.7. With these parameters, the water content in the bottom product of 0.6 mol. The allocation of butyl acetate is carried out at reflux including 1.0 and share selection in the distillate of 0.7. As the cubic product selected butyl acetate content of 99.2% Allocation of butanol is carried out at reflux including 4.0 and share selection in the distillate of 0.8. In Cuba, the column select butanol content is 99.8 mol. Butanol and butyl acetate meet the requirements of GOST.

P R I m e R 4 (beyond the boundaries of separation options). Spent solvents of the composition given in example 1 is subjected to rectification in example 1, but at reflux to column selection of a mixture of butanol and butyl acetate, 0.1, and share selection in the distillate of 0.4. With these parameters, the water content in the bottom product of 1.7 mol. The allocation of butyl acetate is carried out at reflux the number 0.8 and share selection in the distillate of 0.6. As the cubic product selected butyl acetate content is 98.7 wt. The selection of butanol is carried out at reflux cisne meet the requirements of GOST.

METHOD of extraction of BUTANOL, butyl acetate AND WATER FROM the MIXTURE, including the allocation of butanol and butyl acetate in cubes of distillation columns by azeotropic distillation and separation of distillate products of rectification on the water and organic layers in the separators, the recycle stream is used layers of separators, wherein the pre-cleanse is a partial mixture of impurities in a rotary film evaporator with a bit of selection in the distillate is between 0.90 and 0.92, distillates rotary film evaporators rasclaat in the water separators and organic layers, return water layers on irrigation rotary film evaporators, and organic layers emit a mixture of butanol and butyl acetate by azeotropic distillation in Cuba distillation column with reflux from 0.3 to 1.0 and share selection in the distillate from 0.5 to 0.7, obtained when the distillate is rasclaat in the water separator and the organic layer, return the water layer for irrigation of a rotary film evaporator and the organic layer recycle for separation of a mixture of butanol and butyl acetate, butyl acetate extraction is carried out by azeotropic distillation of the mixture of butanol and butyl acetate at flegma azeotropic composition, of which produce butanol by heterotetrameric distillation with water at reflux the number from 4.0 to 5.0 and share selection in the distillate from 0.75 to 0.8, the distillate of the column heterotetramer rectification, consisting of a mixture of water, butanol and butyl acetate, rasclaat in the separator water layer, which return for the allocation of butanol, and the organic layer, which is mixed with an organic layers rotary film evaporators for separation of a mixture of butanol and butyl acetate.

 

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10 cl, 3 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a method of separating a solution of homogeneous catalyst from unrefined monoethylene glycol (MEG) and purifying MEG, for use in catalytic conversion of ethylene oxide (EO) to MEG, where the method involves the following steps: separating the catalyst solution in a catalyst separation section by evaporating unrefined MEG and feeding the unrefined MEG into a rectification section, a section for separating light fractions and from there into a pasteurisation section, where each section works at pressure lower than atmospheric pressure of 0.5105 Nm-2 or lower, where the rectification and pasteurisation sections are at pressure lower than that of the catalyst separation section, where the method provides pressure difference between the catalyst separation section and the rectification section, and where the vapour phase of the unrefined MEG from the catalyst separation section is fed essentially as vapour-phase feed into the rectification section. The invention also relates to apparatus where said method can be realised, as well as use of said method and apparatus in a process or block for catalytic conversion of EO into MEG.

EFFECT: invention enables to reduce the process to a one-run process of evaporating a stream of monoethylene glycol, which enables to transport vapour from the catalyst separation section into the monoethylene glycol purification step without using a mechanical pump.

12 cl, 3 dwg

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