CN102942475A - Variable-pressure rectification method for separating ethyl acetate and ethanol azeotropes and production device for azeotropes - Google Patents
Variable-pressure rectification method for separating ethyl acetate and ethanol azeotropes and production device for azeotropes Download PDFInfo
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Abstract
The invention provides a variable-pressure rectification method for separating ethyl acetate and ethanol azeotropes and a production device for azeotropes. The technological process comprises that an ethyl acetate and ethanol mixture is pumped into a feed pre-heater for preheating, enters a pressurization rectifying tower to be separated, and high-purity ethyl acetate is obtained in a tower reactor; and azeotrope vapor of the ethyl acetate and the ethanol obtained at the tower top is divided into two whiffs, one whiff flows back after being condensed by a condenser, the other whiff is used as a heat source of a constant-pressure rectifying tower, part of the vapor flows back to the top of the constant-pressure rectifying tower after condensation, and the other part returns to the pressurization rectifying tower to be recycled. According to the variable-pressure rectification method for separating ethyl acetate and ethanol azeotropes and the production device for azeotropes, a variable-pressure rectification technology is used, operation can be performed continuously, the technological process is simple, and advantages of low energy and material consumption, high product purity and the like are provided.
Description
Technical field:
The invention belongs to the rectification and purification of chemical field, relate to method and the production unit thereof of a kind of variable-pressure rectification separating ethyl acetate and ethyl alcohol azeotropy article.
Background technology:
Ethyl acetate has another name called vinyl acetic monomer, water white transparency has the liquid of aromatising flavour, have excellent solvability, quick-drying and hypotoxicity, be widely used in the production processes such as coating, tackiness agent, rubber and leatheroid as solvent, being applied to the sepn process of pharmacy and natural product as extraction agent, also is the main raw material of a kind of spices, essence simultaneously.
The production of ethyl method mainly adopts acetic acid and ethyl esterification method at present, ethanol is excessive in the reaction process, ethanol content is about 9% in the ethyl acetate crude product that obtains, if reach " the industrial ethyl acetate of GB/T 3728-2007 " premium grads purity 99.7% requirement, need Re-isolation to purify, but ethyl acetate and ethanol boiling point only differ from 1 ℃ and have azeotropic, azeotropic point is 71.6 ℃ under the normal pressure, ethyl acetate content 0.693(massfraction wherein, lower same), therefore produce high-purity ethyl acetate, can't realize by conventional distillation.At present industrial have azeotropic distillation and extracting rectifying to its separation method.
(1) Chinese patent CN96117836.1 provides the method for a kind of azeotropic distillation separating ethyl acetate and ethanol.The method is take halohydrocarbon as entrainer, and this entrainer does not form azeotrope and forms azeotrope with ethanol with ethyl acetate.The technical process that separates is made of two rectifying tower, and extraction purity is 99.1% ethyl acetate at the bottom of the first rectifying tower, the ethanol of Second distillation column top extraction purity 95%, tower reactor water outlet, the yield 93% of this separating technology ethyl acetate.
(2) chemical engineering institute of Institutes Of Technology Of Hebei has reported use N, the double solvents that dinethylformamide and dimethyl sulfoxide (DMSO) form, adopt batch extracting rectified separating ethyl acetate and ethanol, cat head ethyl acetate product purity reaches 99.5%, use the operating time more required than the use single solvent required extracting rectifying operating time of having a rest of double solvents short, and the unit mass product energy consumption use single solvent low.
(3) Beijing University of Chemical Technology's chemical engineering institute employing ionic liquid is extraction agent, and separation of extractive distillation ethyl acetate and ethanol also carry out flow scheme design, and the result shows that when the ethyl acetate rate of recovery was 98%, ethyl acetate purity was reached for 99.60%.
In the above several method, method (1) belongs to azeotropic distillation, and method (2,3) belongs to extracting rectifying, above-mentioned the deficiencies in the prior art: (1) those method sepn process energy consumptions are all higher; (2) because system is introduced other components, such as extraction agent, entrainer or inorganic salt etc., affected to a certain extent the quality of product; (3) owing to carrying a small amount of ethyl acetate secretly in extraction agent or the entrainer, thereby reduced the yield of product ethyl acetate.
Summary of the invention:
The object of the invention is to overcome the deficiency of above-mentioned technology, method and the production unit thereof of a kind of variable-pressure rectification separating ethyl acetate and ethyl alcohol azeotropy article are provided, the method of this variable-pressure rectification separating ethyl acetate and ethyl alcohol azeotropy article and production unit thereof have not only been realized energy-saving and cost-reducing purpose, and have solved the problems such as product purity, solvent recuperation and energy consumption that azeotropic distillation and extraction rectification technique exist are higher.
The technical scheme that the present invention takes:
The method of variable-pressure rectification separating ethyl acetate of the present invention and ethyl alcohol azeotropy article is characterized in that: the method for variable-pressure rectification separating azeotrope is carried out as follows:
1) ethyl acetate and alcohol mixture enter the compression rectification tower after pumping into the feed preheater preheating, and tower reactor obtains highly purified ethyl acetate after separating; Cat head obtains adding the azeotrope steam of depressing ethyl acetate and ethanol and is divided into two strands, refluxes after the stock-traders' know-how condenser condenses, and another strand is as the thermal source of atmospheric distillation tower, and the condensation rear section is back to the compression rectification top of tower, and another part pumps into the atmospheric distillation tower to be separated;
2) material of compression rectification column overhead extraction pumps into the atmospheric distillation tower, and tower reactor obtains highly purified ethanol after separating; Cat head obtains the azeotrope steam of ethyl acetate and ethanol under the normal pressure after condenser condenses, and a part is back to the atmospheric distillation column overhead, and another part returns compression rectification tower recycled.
The production unit of variable-pressure rectification separating ethyl acetate of the present invention and ethyl alcohol azeotropy article comprises compression rectification tower and atmospheric distillation tower.
Above-mentioned compression rectification tower is tray column or packing tower, is made of rectifying section and stripping section, and wherein theoretical number of plates of rectifying section is 15～25, and the stripping section number of theoretical plate is 10～20; Working pressure is 0.3～1.0MPa(absolute pressure), control of reflux ratio is 2～6; It is 58.2～44.2% that described compression rectification column overhead obtains the ethyl acetate massfraction, and the tower reactor Produced Liquid is the ethyl acetate more than 99.7%.
Above-mentioned atmospheric distillation tower is tray column or packing tower, is made of rectifying section and stripping section, and wherein theoretical number of plates of rectifying section is 15～25, and the stripping section number of theoretical plate is 10～20; Working pressure is normal pressure, and control of reflux ratio is 2～5; It is 69.3% that described atmospheric distillation column overhead obtains the ethyl acetate massfraction, returns compression rectification tower recycled; Tower reactor extraction massfraction is greater than 99.0% methyl alcohol.
The material inlet of above-mentioned compression rectification tower is connected with feed preheater, and discharge port connects the tower reactor reboiler at the bottom of the tower of compression rectification tower, and the azeotrope steam discharge port of compression rectification tower connects overhead condenser; Discharge port connects tower reactor reboiler and trim the top of column pump at the bottom of the tower of described atmospheric distillation tower, and the azeotrope steam discharge port of atmospheric distillation tower connects overhead condenser and trim the top of column pump.
Ultimate principle of the present invention is to utilize the azeotropic composition of ethyl acetate and ethanol with the characteristics of pressure change sensitivity, adopt two different rectifying tower of working pressure to realize the separating-purifying of azeotrope, and integrated by heat, realize energy-saving and cost-reducing purpose, and solved the problems such as product purity, solvent recuperation and energy consumption that present azeotropic distillation and extraction rectification technique exist are higher.Therefore, the present invention has that yield is high, product purity is high, energy consumption is low and the advantage such as technique is simple.
Description of drawings:
Fig. 1 is the production technological process of variable-pressure rectification separating ethyl acetate of the present invention and ethyl alcohol azeotropy article;
Number in the figure is as follows: T1 – compression rectification tower, T2 – atmospheric distillation tower, E01 – T1 feed preheater, E02 – T1 overhead condenser, E04 – T2 overhead condenser, E03 – T1 tower reactor reboiler, E05 – T2 tower reactor reboiler, P01 – T1 trim the top of column pump, P02 – T2 trim the top of column pump, S01 – material feeding tube, S02 – E01 cold material discharge nozzle, S03 – T1 tower reactor extraction pipe, S04 – E01 thermal material discharge nozzle, S05 – T1 overhead vapours pipe, S06 – E02 gas-phase feed pipe, S07 – E05 steam feed pipe, S08 – T1 trim the top of column pipe, S09 – T2 material feeding pipe, S10 – T2 tower reactor extraction pipe, S11 – T2 trim the top of column pipe, S12 – T2 overhead extraction circulation tube.
Embodiment:
Azeotropic among the present invention under ethyl acetate and the ethanol normal pressure consists of: ethyl acetate 0.693, ethanol 0.307; 0.4MPa(the azeotropic absolute pressure) consists of: ethyl acetate 0.549, ethanol 0.451; 0.6MPa(the azeotropic absolute pressure) consists of: ethyl acetate 0.501, ethanol 0.499; 0.8MPa(the azeotropic absolute pressure) consists of: ethyl acetate 0.467, ethanol 0.533.Because normal pressure is depressed the difference that this system azeotropic forms with adding, therefore after ethyl acetate and ethanol are introduced into the compression rectification tower and separate among the present invention, tower reactor obtains high-purity ethyl acetate, cat head obtains adding the azeotrope of depressing ethyl acetate and ethanol, this azeotrope enters the atmospheric distillation tower, tower reactor obtains high-purity ethanol, and cat head obtains that the azeotrope of ethyl acetate and ethanol returns compression rectification tower recycled under the normal pressure.
The present invention is further described below in conjunction with Fig. 1.
Ethyl acetate and ethanol mixing raw material are after the feed preheater E01 preheating of feed-pipe S01 by T1, with enter compression rectification tower T1 after the recycle stock S12 that comes from atmospheric distillation tower T2 cat head mixes and separate, the azeotrope steam S05 that rises in the tower is divided into two strands, wherein one steam S06 refluxes after overhead condenser E02 condensation, another strand steam S07 is as the thermal source of the reboiler E05 of atmospheric distillation tower T2, condensation is back to the compression rectification top of tower by pump P01 pressurization rear section by the S08 materail tube, and another part enters atmospheric distillation tower T2 by the S09 materail tube to be separated; Tower reactor obtains highly purified ethyl acetate and enters preheater E01 preheating material through the S03 materail tube and go out system by the S04 materail tube.
The material of compression rectification column overhead extraction enters atmospheric distillation tower T2 through the S09 materail tube to be separated, cat head obtains the azeotrope steam of ethyl acetate and ethanol under the normal pressure after condenser E04 condensation, be back to the atmospheric distillation column overhead through pump P02 pressurization rear portion by materail tube S11, another part returns compression rectification tower T1 recycled through the S12 materail tube; Tower reactor obtains highly purified ethanol and exports through tower reactor extraction pipe S10.
Embodiment 1:
Adopt the technical process shown in the accompanying drawing 1, feed rate is 1000kg/h, 25 ℃ of feeding temperatures, feed composition: ethyl acetate 91%, ethanol 9%.Compression rectification tower T1 body of the tower material is SUS304, fills CY700 structured wire corrugated wire gauze packing in the tower, and tower diameter is 600mm, number of theoretical plate is 26, the 18 chargings, operational condition: working pressure 0.8MPa, 139.2 ℃ of tower top temperatures, 157.4 ℃ of column bottom temperatures, reflux ratio 5; Atmospheric distillation tower T2 body of the tower material is SUS304, fills CY700 structured wire corrugated wire gauze packing in the tower, and tower diameter is 500mm, and number of theoretical plate is 30, the 22 chargings, operational condition: working pressure 0.1MPa, 72 ℃ of tower top temperatures, 78 ℃ of column bottom temperatures, reflux ratio 4.
Compression rectification tower tower T1 overhead extraction amount is 266.3kg/h, forms: ethyl acetate 0.467, ethanol 0.533; The tower reactor produced quantity is 911.9kg/h, forms: ethyl acetate 0.997, ethanol 0.003.Atmospheric distillation tower tower T2 overhead extraction amount 178.2kg/h forms: ethyl acetate 0.693, ethanol 0.307; The tower reactor produced quantity is 88.1kg/h, forms: ethyl acetate 0.01, ethanol 0.99.
As seen adopt variable-pressure rectification method of the present invention, the purity of ethyl acetate reaches 99.7% behind the separating-purifying, and yield reaches 99.8%.
Embodiment 2:
Adopt the technical process shown in the accompanying drawing 1, feed rate is 1000kg/h, 25 ℃ of feeding temperatures, feed composition: ethyl acetate 91%, ethanol 9%.Compression rectification tower T1 body of the tower material is SUS304, fills BX500 structured wire corrugated wire gauze packing in the tower, and tower diameter is 500mm, number of theoretical plate is 30, the 20 chargings, operational condition: working pressure 0.6MPa, 128.3 ℃ of tower top temperatures, 144.1 ℃ of column bottom temperatures, reflux ratio 5; Atmospheric distillation tower T2 body of the tower material is SUS304, fills BX500 structured wire corrugated wire gauze packing in the tower, and tower diameter is 400mm, and number of theoretical plate is 36, the 24 chargings, operational condition: working pressure 0.1MPa, 72 ℃ of tower top temperatures, 78 ℃ of column bottom temperatures, reflux ratio 4.5.
Compression rectification tower tower T1 overhead extraction amount is 313.6kg/h, forms: ethyl acetate 0.501, ethanol 0.499; The tower reactor produced quantity is 911.9kg/h, forms: ethyl acetate 0.997, ethanol 0.003.Atmospheric distillation tower tower T2 overhead extraction amount is 225.4kg/h, forms: ethyl acetate 0.693, ethanol 0.307; The tower reactor produced quantity is 88.1kg/h, forms: ethyl acetate 0.01, ethanol 0.99.
Embodiment 3:
Adopt the technical process shown in the accompanying drawing 1, feed rate is 1500kg/h, 25 ℃ of feeding temperatures, feed composition: ethyl acetate 91%, ethanol 9%.Compression rectification tower T1 body of the tower material is SUS304, fills CY700 structured wire corrugated wire gauze packing in the tower, and tower diameter is 800mm, and number of theoretical plate is 30, the 20 chargings, operational condition: working pressure 0.4MPa, 114 ℃ of tower top temperatures, 127 ℃ of column bottom temperatures, reflux ratio 4.5; Atmospheric distillation tower T2 body of the tower material is SUS304, fills CY700 structured wire corrugated wire gauze packing in the tower, and tower diameter is 600mm, and number of theoretical plate is 36, the 24 chargings, operational condition: working pressure 0.1MPa, 72 ℃ of tower top temperatures, 78 ℃ of column bottom temperatures, reflux ratio 4.
Compression rectification tower tower T1 overhead extraction amount is 627.2kg/h, forms: ethyl acetate 0.549, ethanol 0.451; The tower reactor produced quantity is 1367.8kg/h, forms: ethyl acetate 0.997, ethanol 0.003.Atmospheric distillation tower tower T2 overhead extraction amount is 494.9kg/h, forms: ethyl acetate 0.693, ethanol 0.307; The tower reactor produced quantity is 132.2kg/h, forms: ethyl acetate 0.01, ethanol 0.99.
As seen adopt variable-pressure rectification method of the present invention, the purity of ethyl acetate reaches 99.7% behind the separating-purifying, and yield reaches 99.8%.
The present invention utilizes the azeotropic composition of ethyl acetate and ethanol with the characteristics of pressure change sensitivity, adopt two different rectifying tower of working pressure to realize the separating-purifying of azeotrope, and integrated by heat, realize energy-saving and cost-reducing purpose, and solved the problems such as product purity, solvent recuperation and energy consumption that present azeotropic distillation and extraction rectification technique exist are higher.Therefore, the present invention has that yield is high, product purity is high, energy consumption is low and the advantage such as technique is simple.
The above only is preferred embodiment of the present invention, and all equalizations of doing according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Claims (5)
1. the method for a variable-pressure rectification separating ethyl acetate and ethyl alcohol azeotropy article, it is characterized in that: the method for variable-pressure rectification separating azeotrope is carried out as follows:
1) ethyl acetate and alcohol mixture enter the compression rectification tower after pumping into the feed preheater preheating, and tower reactor obtains highly purified ethyl acetate after separating; Cat head obtains adding the azeotrope steam of depressing ethyl acetate and ethanol and is divided into two strands, refluxes after the stock-traders' know-how condenser condenses, and another strand is as the thermal source of atmospheric distillation tower, and the condensation rear section is back to the compression rectification top of tower, and another part pumps into the atmospheric distillation tower to be separated;
2) material of compression rectification column overhead extraction pumps into the atmospheric distillation tower, and tower reactor obtains highly purified ethanol after separating; Cat head obtains the azeotrope steam of ethyl acetate and ethanol under the normal pressure after condenser condenses, and a part is back to the atmospheric distillation column overhead, and another part returns compression rectification tower recycled.
2. production unit of realizing the described variable-pressure rectification separating ethyl acetate of claim 1 and ethanol, it is characterized in that: described production unit comprises compression rectification tower and atmospheric distillation tower.
3. the production unit of described variable-pressure rectification separating ethyl acetate and ethanol according to claim 2, it is characterized in that: described compression rectification tower is tray column or packing tower, be made of rectifying section and stripping section, wherein theoretical number of plates of rectifying section is 15～25, and the stripping section number of theoretical plate is 10～20; Working pressure is 0.3～1.0MPa(absolute pressure), control of reflux ratio is 2～6; It is 58.2～44.2% that described compression rectification column overhead obtains the ethyl acetate massfraction, and the tower reactor Produced Liquid is the ethyl acetate more than 99.7%.
4. according to claim 2 or the production unit of 3 described variable-pressure rectification separating ethyl acetates and ethanol, it is characterized in that: described atmospheric distillation tower is tray column or packing tower, be made of rectifying section and stripping section, wherein theoretical number of plates of rectifying section is 15～25, and the stripping section number of theoretical plate is 10～20; Working pressure is normal pressure, and control of reflux ratio is 2～5; It is 69.3% that described atmospheric distillation column overhead obtains the ethyl acetate massfraction, returns compression rectification tower recycled; Tower reactor extraction massfraction is greater than 99.0% methyl alcohol.
5. the production unit of described variable-pressure rectification separating ethyl acetate and ethanol according to claim 2, it is characterized in that: the material inlet of described compression rectification tower is connected with feed preheater, discharge port connects the tower reactor reboiler at the bottom of the tower of compression rectification tower, and the azeotrope steam discharge port of compression rectification tower connects overhead condenser; Discharge port connects tower reactor reboiler and trim the top of column pump at the bottom of the tower of described atmospheric distillation tower, and the azeotrope steam discharge port of atmospheric distillation tower connects overhead condenser and trim the top of column pump.
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Effective date of registration: 20161230 Address after: Jishan Industrial Park 353399 Sanming City Jiangle County in Fujian Province Economic Development Zone Patentee after: Fujian Hongyan Chemical Co., Ltd. Address before: 350300 Fuqing, Fujian, Longjiang, Fuzhou Street Village, No. 1 Patentee before: Fuqing Branch of Fujian Normal University |