Method of producing dehydrated ethyl alcohol

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of producing dehydrated ethyl alcohol, which can be used in chemical, electronic and pharmaceutical industry. The method involves feeding crude alcohol or a water-alcohol solution into a preliminary dehydration column operating under a vacuum to obtain a distillate which is fed into a final dehydration column operating at excess pressure, where dehydrated alcohol is collected in form of a residue and the distillate is fed into the preliminary dehydration column in form of reflux. The distillation process in the preliminary dehydration column takes place at absolute pressure of 8.0-13.3 kPa to obtain a distillate with alcohol content 98.2-98.9 vol. %, and the distillation process in the final dehydration column takes place at absolute pressure 0.1-0.5 MPa and alcohol content in the reflux of 96.5-97.2 vol. %.

EFFECT: method enables to obtain an end product of high quality using an improved an improved process scheme.

1 tbl, 1 dwg, 2 ex

 

The invention relates to the alcohol industry, namely the production of dehydrated ethyl alcohol (absolute), and can be used in chemical, electronic, pharmaceutical industry.

Known processes for the dehydration of ethanol, based on the use of chemical methods, and various processes, such as extraction, adsorption, azeotropic and extractive distillation, pervaporation.

One of the ways to obtain absolute ethyl alcohol is getting dehydrated ethyl alcohol, with the separation of mixtures in complex distillation columns operating at different pressures. The basis of this method is supposed to change the content of ethyl alcohol in the azeotropic mixture ethanol - water depending on the pressure.

To get dehydrated ethyl alcohol presents a possible technological scheme of the two-column installation (Swillow. Some questions rectification of binary and multicomponent mixtures. M.: Izd. Academy of Sciences of the USSR, 1960, s). In the first column, operating under atmospheric pressure, from a source, poor ethanol mixture, is obtained as a bottom product and water as the top product is a mixture, similar to the composition of the azeotrope, i.e 90 mol.% ethyl alcohol and 10 mol.% water. The last pump is pumped into the WTO the second distillation column, working under pressure of 75 ATM (about 7.6 MPa), where as the top product will Athanasia mixture similar in composition to the azeotropic mixtures with a content of 70 mol.% ethyl alcohol and 30 mol.% water, which is re-directed to the enrichment in the first column, and the lower product will get a little dehydrated alcohol.

Known technological scheme of production of bio-ethanol used as fuel ethanol, including scheme dehydration, consisting of two columns (N.Arifeen, R.Wang, I..Kookos, .Webb, A.A.Koutinas. Process design and optimization of novel wheat-based continuous bioethanol production system. Biotechnol. Prog. 2007, 23, 1394-1403). In the first column, pressure 1 bar (0.1 MPa), served the initial mixture containing 40 mol.% ethyl alcohol, where selected distillate containing 89,75 mol.% ethyl alcohol, and waste liquid is water with ethyl alcohol content of 1.09 mol.%. The distillate from the first column is sent to a second column operating pressure 10 bar (1.0 MPa), which in the form of a bottom liquid is drawn dehydrated ethanol containing a 99.0 mol.% ethyl alcohol, and the distillate containing 84,95%) molar ethyl alcohol, which is returned to the first column.

There is a method of dehydration of alcohol (U.S. patent No. 1676700, B01D, publ. 10.07.1928), including the concentration of an aqueous solution of ethyl alcohol containing less than 95.6% of ETANA is a, fractional distillation at an absolute pressure of not more than 6 inch Hg (20,3 KPa) with the selection of distillate containing more than 95.6% of ethanol, and fractional distillation of this distillate at a pressure of at least 100 psi (0,69 MPa) with subsequent removal of dewatered residue and obtain a distillate containing less than 95.6% of ethanol, which is an aqueous solution of ethyl alcohol is fed to the distillation under vacuum.

A method of obtaining digidratirovannogo alcohol from a fermented mash containing 8-10% vol. alcohol (French patent No. 2461751, B01D 3/00, publ. 06.02.1981). Fermented wort, preheated in the heat exchanger is fed to a first distillation column operating under a residual pressure of 190 mm Hg (25,3 KPa) in the head part. The alcohol concentration of 97.4 wt.%, selected and directed by a pump through a heat exchanger in a distillation column which operates at a pressure of 7 bar (0.7 MPa). At this pressure the alcohol content in the azeotrope of the alcohol - water is 93,6 wt.% thus, the power of this column can be considered as pseudobinary a mixture of 40.6 wt.% azeotropic mixtures (the easier part) and 59.4 wt.% anhydrous alcohol (the hard part). Absolute alcohol is withdrawn from the base of the second column and is cooled. Azeotropic mixture with 10% absolute ethanol is removed from the head h is STI the second column and is returned in the first column. Highlighted in the head part of the second column pair is compressed up to 7-8 bar (0,7-0,8 MPa) compressor driven by a steam turbine. Compressed alcohol vapors are condensed in a heat exchanger, heating the second column. Output digidratirovannogo alcohol is about 97% based on the alcohol feedstock.

The above technological schemes of getting dehydrated ethyl alcohol using distillation columns, pressure, require the use of high pressure steam or other high temperature heat transfer fluids to ensure that the specified parameters of the process of rectification column of high pressure, which increases the consumption of heat flow meters, as well as creating a separation of complexes using devices of various functional steps, which complicates the technological scheme of production.

The aim of the present invention is an improvement of the method of dehydration of alcohol, improving the quality of the target product.

This objective is achieved in that the method of producing ethyl alcohol absolute includes the supply of crude alcohol or water-alcohol solution in the column pre-dehydration, working under vacuum to obtain a distillate, which is sent to the final dehydration column operating at a pressure, which is selected absolute alcohol in the form of a bottom liquid and distillate in the form of return flow is directed to the column pre-dehydration. The process of rectification column pre-dehydration is carried out at an absolute pressure of 8.0-13.3 KPa to obtain a distillate with alcohol content of 98.2 reached 98.9%, and the process of rectification in the column of final dehydration is carried out at an absolute pressure of 0.1-0.5 MPa, and the alcohol content in the outlet stream of 96.5-97,2%vol.

The proposed method allows to significantly simplify the technological scheme of dehydration of alcohol, namely to abandon sophisticated equipment for mechanical vapor recompression. The process is conducted at a lower pressure, which reduces the requirements to the characteristics of fluids, can easily implement this method in distilleries that use in the industrial cycle water vapor 0.6 MPa, and to guarantee receipt of ethyl alcohol absolute fortress of 99.5-99,95%vol.

The method of obtaining absolute ethyl alcohol is carried out at the facility, the scheme of which is shown in the drawing, as follows.

Raw materials (alcohol 95% vol. or water-alcohol solution of a strength of 40%vol.) taken in collection 1. From collection 1 raw line 2 is fed into the column 3 in the px first or second (counting from the bottom) drawer sides columns 3 due to the pressure difference in collection 1 (atmospheric) and column 3 (vacuum). Column 3 is the preliminary dehydration of the alcohol under vacuum at an absolute pressure of 8.0-13.3 KPa. Column 3 has 5 rings it is filled with regular packing of metal mesh, equipped with a reflux condenser 4 and the condenser 5, the cooled water with a temperature of 5-7C. the Heating of the column 3 is performed through a remote boiler 6 water vapor. A pair coming from the column 3, is condensed in the reflux condenser 4 and the capacitor 5 and flegma the collector phlegmy 7 return to top of square section column 3. Non-condensable vapors and gases from the condenser 5 are received in the vacuum manifold (not shown). The distillate, which is partially dehydrated alcohol level 98.2 reached 98.9%, is taken from the collector of phlegmy 7 barometric pipe 8 into the collector 9, under atmospheric pressure. Its bottom liquid of the column 3 (Lucerna water) is given in vakuumirovaniya collection 10.

From collection 9 partially dehydrated alcohol by pump 11 through line 12 through the heater 13 is fed into the column 14 to the top of the second or third (counting from the bottom), side bars of the column 14. The heater 13, the heating which is carried out with steam, partially dehydrated alcohol is heated to a temperature of 95-100C. the column 14 is the final dehydration of alcohol at an absolute pressure of 0.1-0.5 MPa. Column 14 has 5 bars, filled controllers is Noah nozzle of metal mesh, equipped with reflux condenser 15, water cooled. Heating of the column 14 is made through a remote boiler 16 water vapor. A pair coming from the column 14, are condensed in the reflux condenser 15 and flegma the collector phlegmy 17 return to top of square section columns 14. Air line 18 to column 15 is equipped with a safety valve (not shown). The distillate of the column 14, which is the recurrent alcohol 96,5-97,2%, is taken from the collector of phlegmy 17 and is directed through the condenser 19, which is cooled with water to 30C, line 20 to column 3 on top of the second (counting from the bottom), side bars of the column 3 by the difference in pressures in columns 3 and 14. Its bottom liquid of the column 14, which is dehydrated by alcohol 99,5-99,95%, play through the condenser 21, the cooled water in the collector 22 due to the pressure difference in the column 14 (excess) and in the collection 22 (naturally).

The modes of operation of distillation columns and the quality of absolute ethyl alcohol by the proposed method are presented in the table.

/tr>
Mode columnsExample 1Example 2
Consumption of raw materials, kg/h100100
The alcohol content in the feedstock,% vol.4095
Column pre-dehydration
Pressure, KPa13,38.0
The temperature of the top of the column, C34,325,2
The temperature of the cube column, C56,848,7
The alcohol content in the distillate,% vol.of 98.2the 98.9
The alcohol content in the bottom of fluids, vol.%0,10,5
Consumption of distillate, kg/h77,8135,7
The bottom flow of the fluid, kg/h66,57,5
Column final dehydration
Pressure, MPa0,10,5
The temperature of the top of the column, C78,1125,1
The temperature of the cube column, C79,2126,0
The alcohol content in the distillate (return flow), vol.%97,296,5
The alcohol content in the bottom liquid (absolute alcohol), vol.%99.5at 99.95
Consumption of distillate (return flow), kg/h44,343,2
The flow rate of the bottom liquid (absolute alcohol), kg/h33,592,5

The method of producing ethyl alcohol absolute, including the supply of crude alcohol or water-alcohol solution in the column pre-dehydration, working under vacuum to obtain a distillate, which is sent to the final dehydration column operating at a pressure at which the selected absolute alcohol in the form of a bottom liquid and distillate in the form of return flow is directed to the column pre-dehydration, Otley is audica fact, the process of rectification column pre-dehydration is carried out at an absolute pressure of 8.0-13.3 KPa to obtain a distillate with alcohol content of 98.2 reached 98.9%, and the process of rectification in the column of final dehydration is carried out at an absolute pressure of 0.1-0.5 MPa, and the alcohol content in the outlet stream of 96.5-97,2%.



 

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