CN110878006B - Method and device for separating ethanol and ethyl acetate - Google Patents
Method and device for separating ethanol and ethyl acetate Download PDFInfo
- Publication number
- CN110878006B CN110878006B CN201811033769.8A CN201811033769A CN110878006B CN 110878006 B CN110878006 B CN 110878006B CN 201811033769 A CN201811033769 A CN 201811033769A CN 110878006 B CN110878006 B CN 110878006B
- Authority
- CN
- China
- Prior art keywords
- tower
- ethanol
- ethyl acetate
- separation
- separator
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Abstract
The invention relates to the field of separation of ethanol and ethyl acetate, and discloses a method and a device for separating ethanol and ethyl acetate, wherein the method comprises the following steps: 1) distilling and separating the material to be separated containing ethanol and ethyl acetate in an ethanol separation tower to obtain a second distillate at the tower top and a second residue mainly containing ethanol and water at the tower bottom; rectifying the second residue in an ethanol rectifying tower to obtain ethanol at the tower top; 2) mixing and contacting the second distillate and water in a separator at the top of the ethanol separation tower for extraction and separation to obtain a water phase and an oil phase; 3) and (3) rectifying the oil phase in an ethyl acetate rectifying tower to obtain a fourth distillate at the tower top and ethyl acetate at the tower bottom. The method and the device for separating the ethanol from the ethyl acetate can simultaneously obtain high-purity ethanol and ethyl acetate products, and meet the product quality requirements of industrial alcohol and industrial ethyl acetate.
Description
Technical Field
The invention relates to the field of separation of ethanol and ethyl acetate, in particular to a method and a device for separating ethanol and ethyl acetate.
Background
Ethanol is an important bulk chemical, can be used as vehicle fuel when added into gasoline, and has increasingly large demand for ethanol in China. At present, the ethanol production mainly adopts a fermentation method, and the fermentation method has the problems of high cost and land competition with grains and people. Therefore, the development of coal-to-ethanol will have a great impact on the overall energy market and structural changes. The coal-based ethanol mainly has three routes: (1) preparing ethanol by using synthesis gas in one step. The synthesis gas is produced by coal gasification, the synthesis gas is used for preparing low carbon alcohol by one step method, and the ethanol is separated from the mixed low carbon alcohol. (2) And (3) hydrogenation of acetic ester to prepare ethanol. Gasifying to produce synthetic gas, preparing methanol from the synthetic gas, preparing acetic acid from methanol by carbonylation, preparing acetic ester by esterifying the acetic acid and ethanol, and hydrogenating the acetic ester to obtain the ethanol. (3) The acetic acid is directly hydrogenated to prepare the ethanol. Compared with the acetic ester hydrogenation route, the route for preparing the ethanol by directly hydrogenating the acetic acid has relatively simple process, and technically keys are an efficient acetic acid hydrogenation catalyst, a reactor for controlling a high exothermic reaction and product separation.
In addition, ethyl acetate is an important organic chemical raw material with wide application, has large production capacity, can be used for preparing phthalide amine, acetic acetate, methyl heptenone and the like, and has wide application in the industries of spices, medicines, paint coatings, printing ink and foods. At present, the main production method in China is to react acetic acid with ethanol under the catalysis of concentrated sulfuric acid, and then deacidify, dehydrate and refine the product.
Whether ethanol or ethyl acetate is produced, acetic acid, ethanol, ethyl acetate and other by-products are contained in the crude product. The product water and ethanol can form binary and ternary azeotrope with ethyl acetate, and are partially soluble at normal temperature, and for the direct hydrogenation of acetic acid to prepare ethanol, the content of ethyl ester in the product is low, and is below 10%, and basically all azeotrope is formed, so that the separation from a crude product is difficult.
CN102414153A discloses a process for purifying a crude ethanol product, comprising the steps of: hydrogenating an acetic acid feed stream in a reactor in the presence of a catalyst to form a caide ethanol product; separating at least a portion of the caide ethanol product in a first column into a first distillate comprising ethanol, water, and ethyl acetate, and a first residue comprising acetic acid; separating at least a portion of the first distillate in a second column into a second distillate comprising ethyl acetate and a second residue comprising ethanol and water, wherein the second column is an extractive distillation column; feeding an extractant into the second column; and separating at least a portion of the second residue in a third column into a third distillate comprising ethanol and a third residue comprising water. The method disclosed therein mainly aims at obtaining product ethanol, and the extractant of the used extractive distillation tower is introduced into the extractive distillation tower by using the third tower residue, so that the reflux ratio of the extractive distillation tower is larger, the load of the tower is larger, the ethyl acetate concentration at the tower top is lower, later, if ethyl acetate with high concentration is obtained, the flow path is longer, and the ethyl acetate concentration in the extractive distillation tower residue is increased, therefore, if the third tower is used for obtaining ethanol with high concentration, the number of tower plates and the reflux ratio are increased, and the equipment investment is increased.
CN102421522A discloses a method for recovering ethyl acetate solvent, which comprises the following steps: hydrogenating acetic acid in a reactor in the presence of a catalyst to form a crude product; separating at least a portion of the crude product in a first column into a first distillate comprising ethanol, water, and ethyl acetate, and a first residue comprising acetic acid, wherein the first residue comprises substantially all of the acetic acid from the at least a portion of the crude product; and separating at least a portion of the first distillate to form an ethyl acetate solvent comprising ethyl acetate and ethanol. The method further comprises the following steps: separating at least a portion of the first distillate in a second column into a second distillate comprising ethyl acetate solvent and a second residue comprising water, separating at least a portion of the second residue in a third column into a third distillate comprising ethanol and a third residue comprising water, and separating at least a portion of the second distillate in a fourth column into a fourth distillate comprising acetaldehyde and a fourth residue comprising ethyl acetate solvent. The method disclosed in CN102421522A still cannot avoid the problems of large reflux ratio and large tower load; in addition, the obtained ethyl acetate product is an ethyl acetate solvent containing ethanol, and ethyl acetate with higher purity cannot be obtained.
Disclosure of Invention
The invention aims to solve the problems of large reflux and large tower load in the separation process of ethanol and ethyl acetate in the prior art, and provides a method and a device for separating ethanol and ethyl acetate. The method for separating the ethanol from the ethyl acetate can reduce equipment investment, shorten the process flow and reduce energy consumption.
In a first aspect, the present invention provides a process for the separation of ethanol and ethyl acetate, the process comprising:
1) distilling and separating the material to be separated containing ethanol and ethyl acetate in an ethanol separation tower to obtain a second distillate at the tower top and a second residue mainly containing ethanol and water at the tower bottom; rectifying the second residue in an ethanol rectifying tower to obtain ethanol at the tower top;
2) mixing and contacting the second distillate and water in a separator at the top of the ethanol separation tower for extraction and separation to obtain a water phase and an oil phase;
3) and (3) rectifying the oil phase in an ethyl acetate rectifying tower to obtain a fourth distillate at the tower top and ethyl acetate at the tower bottom.
Preferably, the third residue obtained from the bottom of the ethanol rectification column is introduced into an ethanol separation column overhead separator to provide the water.
In a second aspect, the present invention provides an apparatus for separating ethanol from ethyl acetate, the apparatus comprising:
the ethanol separation tower is used for distilling and separating the materials to be separated containing ethanol and ethyl acetate, a second distillate is obtained at the tower top, and a second residue mainly containing ethanol and water is obtained at the tower bottom;
the ethanol rectifying tower is used for rectifying the second residue to obtain ethanol at the tower top;
the ethanol separation tower top separator is used for mixing and contacting the second distillate and water for extraction and separation to obtain a water phase and an oil phase;
and the ethyl acetate rectifying tower is used for rectifying the oil phase to obtain a fourth distillate at the tower top and ethyl acetate at the tower bottom.
Preferably, the bottom outlet of the ethanol rectification column is in communication with the inlet of the ethanol separation column overhead separator such that the third residue is returned to the ethanol separation column overhead separator.
The method and the device for separating the ethanol from the ethyl acetate can simultaneously obtain high-purity ethanol and ethyl acetate products, and meet the product quality requirements of industrial alcohol and industrial ethyl acetate. The invention can obtain higher purity products by reasonably arranging the top separator of the ethanol separation tower, in addition, under the optimal condition, the invention reduces the circulating water quantity of the system, reduces the tower plate number and the reflux ratio, reduces the separation energy consumption and improves the product yield. The method for separating the ethanol from the ethyl acetate and the device thereof reasonably set the ethanol separation tower and the top separator of the ethanol separation tower to improve the product purity have relatively small influence on the number of tower plates and the reflux ratio, and different tower top concentrations can meet the requirement of product separation by adjusting the amount of added water.
Drawings
FIG. 1 is a schematic diagram of the separation apparatus for ethanol and ethyl acetate provided in example 1;
FIG. 2 is a schematic view of the apparatus for separating ethanol and ethyl acetate provided in comparative example 1.
Description of the reference numerals
1-acetic acid separation tower, 2-ethanol separation tower and 3-ethanol rectifying tower
4-ethyl acetate rectifying tower 5-heat exchanger 6-cooler
7-first condenser 8-second condenser 9-ethanol separation tower top separator
10-side line separator 11-gas-liquid separator
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating the invention, are intended for purposes of illustration and explanation only and are not intended to limit the scope of the invention.
In the present invention, the use of directional terms such as "top, bottom, side" and "lateral" generally refer to the top, bottom and side as generally described and illustrated in the figures.
In the present invention, for the sake of convenience of distinction, the stream obtained at the top of the column is referred to as a distillate, and the stream obtained at the bottom of the column is referred to as a residue.
The invention provides a method for separating ethanol and ethyl acetate, which comprises the following steps:
1) distilling and separating the materials to be separated containing ethanol and ethyl acetate in an ethanol separation tower 2 to obtain a second distillate at the tower top and a second residue mainly containing ethanol and water at the tower bottom; rectifying the second residue in an ethanol rectifying tower 3 to obtain ethanol at the tower top;
2) mixing and contacting the second distillate and water in a tower top separator 9 of an ethanol separation tower for extraction and separation to obtain a water phase and an oil phase;
3) and (3) rectifying the oil phase in an ethyl acetate rectifying tower 4 to obtain a fourth distillate at the tower top and ethyl acetate at the tower bottom.
In the present invention, the terms "first", "second", "third" and "fourth" are used for distinguishing different devices and/or components without limiting the specific contents of the devices and/or components.
The ethanol separation tower 2 is used for separating ethanol from materials to be separated, a second residue mainly containing ethanol and water is obtained at the bottom of the tower, and ethanol, water, ethyl acetate, acetaldehyde and other light components are arranged at the top of the tower.
According to a preferred embodiment of the present invention, the conditions for the distillation separation in the ethanol separation column 2 include: the temperature at the top of the tower is 20-70 ℃, the pressure at the top of the tower is 0.01-0.1MPa, the temperature at the bottom of the tower is 60-88 ℃, the pressure at the bottom of the tower is 0.04-0.13MPa, the number of tower plates is 20-32, and the reflux ratio is 3-8; further preferably, the temperature at the top of the column is 50-65 ℃, the pressure at the top of the column is 0.04-0.08MPa, the temperature at the bottom of the column is 75-85 ℃, the pressure at the bottom of the column is 0.07-0.13MPa, the number of the column plates is 26-32, and the reflux ratio is 4-7.
In the invention, the second distillate obtained from the top of the ethanol separation tower 2 enters an ethanol separation tower top separator 9 to be mixed and contacted with water for extraction separation, and in order to further obtain ethanol with higher purity, the second residue mainly containing ethanol and water obtained from the bottom of the ethanol separation tower 2 is sent to an ethanol rectifying tower 3 for rectification, the product ethanol is obtained from the top of the tower, and the third residue (containing water and a small amount of ethanol) is obtained from the bottom of the tower.
According to a preferred embodiment of the present invention, the conditions for rectification in ethanol rectification column 3 include: the temperature at the top of the tower is 30-78 ℃, the pressure at the top of the tower is 0.01-0.1MPa, the temperature at the bottom of the tower is 74-104 ℃, the pressure at the bottom of the tower is 0.04-0.13MPa, the number of tower plates is 29-40, and the reflux ratio is 10-20; further preferably, the temperature of the top of the column is 60-78 ℃, the pressure of the top of the column is 0.06-0.1MPa, the temperature of the bottom of the column is 94-104 ℃, the pressure of the bottom of the column is 0.08-0.13MPa, the number of the tower plates is 34-38, and the reflux ratio is 13-18.
According to an embodiment of the present invention, the second distillate may be condensed (preferably to 20 to 30 ℃) by the first condenser 7 and then passed into the ethanol separation column overhead separator 9.
According to a preferred embodiment of the present invention, the conditions for the extractive separation in the overhead separator 9 of the ethanol separation column include: the temperature is 20-30 ℃, and the pressure is 0.01-0.1 MPa.
According to a preferred embodiment of the invention, the mass ratio of water to the second distillate in ethanol in step 2) is from 2 to 18: 1.
The water used in step 2) of the present invention may be fresh water or recyclable water used in the method provided by the present invention. According to a preferred embodiment of the present invention, the third residue obtained at the bottom of the ethanol rectification column 3 is introduced into an ethanol separation column overhead separator 9 to provide said water. With this preferred embodiment, the water in the system is fully utilized, reducing the use of fresh water. From the above, one skilled in the art can determine, based on the amount of water required in the ethanol separation column overhead separator 9, whether to introduce all of the third residue into the ethanol separation column overhead separator 9 to provide the water or to introduce a portion of the third residue into the ethanol separation column overhead separator 9 to provide the water. If a portion of the third residue is introduced into the ethanol separation column overhead separator 9, the remaining portion of the third residue may be discharged.
The material in the overhead separator 9 of the ethanol separation column is separated into an aqueous phase and an oil phase, and preferably, the aqueous phase is returned to the ethanol separation column 2 in step 2). This preferred embodiment allows further separation of the ethanol in the aqueous phase.
According to the invention, the oil phase obtained in the top separator 9 of the ethanol separation column is rectified in the ethyl acetate rectification column 4 in order to separate the ethyl acetate in the oil phase (obtained at the bottom of the ethyl acetate rectification column 4).
According to a preferred embodiment of the present invention, the conditions for rectification in ethyl acetate rectification column 4 include: the temperature at the top of the tower is 47-64 ℃, the pressure at the top of the tower is 0.04-0.08MPa, the temperature at the bottom of the tower is 62-77 ℃, the pressure at the bottom of the tower is 0.06-0.1MPa, the number of tower plates is 18-26, and the reflux ratio is 3-8; further preferably, the temperature at the top of the column is 55-64 ℃, the pressure at the top of the column is 0.06-0.08MPa, the temperature at the bottom of the column is 68-77 ℃, the pressure at the bottom of the column is 0.06-0.1MPa, the number of the column plates is 20-24, and the reflux ratio is 4-8.
The fourth distillate obtained from the top of the ethyl acetate rectifying tower 4 mainly contains acetaldehyde, ethyl acetate and part of ethanol, and in order to further improve the product yield, the method preferably further comprises the following steps: and carrying out gas-liquid separation on the fourth distillate in a gas-liquid separator 11, wherein a gas phase mainly containing acetaldehyde is obtained at the top of the gas-liquid separator 11, and a liquid phase mainly containing ethyl acetate and ethanol is obtained at the bottom of the gas-liquid separator 11.
According to an embodiment of the present invention, the condition for performing gas-liquid separation in the gas-liquid separator 11 includes: the temperature is 40-50 deg.C, and the pressure is 0.04-0.08 MPa.
According to an embodiment of the present invention, the gas-liquid separation may be performed by condensing the fourth distillate after passing through the second condenser 8 (preferably, to 40 to 50 ℃).
According to an embodiment of the present invention, the liquid phase mainly containing ethyl acetate and ethanol may be returned to the overhead separator 9 of the ethanol separation column to further separate and utilize ethyl acetate and ethanol therein.
According to a preferred embodiment of the invention, the method further comprises: a side stream is taken from the side of the ethyl acetate rectification column 4. A side stream may be taken in the upper middle portion of the column.
Preferably, the extraction temperature is 51-66 ℃ and the pressure is 0.05-0.09 MPa. The composition of the side stream is not particularly limited in the present invention and may contain, for example, 87 to 91 wt% ethyl acetate, 6 to 8 wt% water, 2 to 4 wt% ethanol.
According to a preferred embodiment of the present invention, the side stream and water (preferably fresh water) are mixed and contacted in a side separator 10 for extractive separation to obtain an aqueous phase (discharge) and an oil phase; further preferably, the oil phase separated in the side line separator 10 is returned to the ethyl acetate rectification column 4. This preferred embodiment is more advantageous in increasing the yield of ethyl acetate. Preferably, the temperature of the extractive separation is not higher than 45 ℃, for example 20-45 ℃.
According to a preferred embodiment of the invention, the mass ratio of water added in the side-line separator 10 to the side stream in terms of ethanol is in the range of from 5 to 20:1, more preferably in the range of from 10 to 15: 1.
According to the method provided by the invention, preferably, when the material to be separated also contains acetic acid, the method also comprises the step of separating the acetic acid from the material to be separated, and then carrying out the step 1).
According to the method provided by the invention, preferably, the material to be separated also contains acetic acid, and the method further comprises the following steps: distilling and separating the materials to be separated in an acetic acid separation tower 1 to obtain a first distillate at the tower top and a first residue mainly containing acetic acid and water at the tower bottom, and carrying out the distillation and separation on the first distillate in an ethanol separation tower 2.
According to the method provided by the invention, the material to be separated is preferably preheated (can be preheated to 50-60 ℃) and then sent to the acetic acid separation tower 1 for distillation separation. In order to effectively utilize the heat source in the system, the method preferably further comprises the step of exchanging heat of the third residue obtained at the bottom of the ethanol rectifying tower 3 and the material to be separated by using a heat exchanger 5. This preferred embodiment enables preheating of the material to be separated by means of the heat of the third residue.
According to one embodiment of the present invention, the process further comprises cooling the heat exchanged third residue with a cooler 6 (preferably to 20-50 ℃) and then feeding the cooled third residue to an overhead separator 9 of an ethanol separation column.
According to a preferred embodiment of the present invention, the conditions for the distillation separation in the acetic acid separation column 1 include: the temperature at the top of the tower is 35-90 ℃, the pressure at the top of the tower is 0.01-0.11MPa, the temperature at the bottom of the tower is 97-130 ℃, the pressure at the bottom of the tower is 0.06-0.16MPa, the number of tower plates is 16-27, and the reflux ratio is 2.5-5; further preferably, the temperature at the top of the column is 75 to 85 ℃, the pressure at the top of the column is 0.06 to 0.1MPa, the temperature at the bottom of the column is 115 ℃ to 125 ℃, the pressure at the bottom of the column is 0.1 to 0.15MPa, the number of the plates is 20 to 24, and the reflux ratio is 3 to 5.
The process provided by the present invention is applicable to any material to be separated containing ethanol and ethyl acetate, and optionally acetic acid. The content of ethanol, ethyl acetate and acetic acid in the material to be separated is not particularly limited, and preferably, the content of ethanol in the material to be separated is 45-70 wt%, the content of ethyl acetate in the material to be separated is 1-20 wt%, the content of water in the material to be separated is 10-35 wt%, the content of acetic acid in the material to be separated is 0-20 wt%, the content of acetaldehyde in the material to be separated is 0-3 wt%, and the total content of n-propanol and acetone in the material to be separated is 0-2 wt%. The method provided by the invention is particularly suitable for separating ethanol and ethyl acetate from the material to be separated with the composition.
The invention also provides a device for separating ethanol from ethyl acetate, which comprises: the ethanol separation tower 2 is used for distilling and separating the materials to be separated containing ethanol and ethyl acetate to obtain a second distillate at the tower top and a second residue mainly containing ethanol and water at the tower bottom;
the ethanol rectifying tower 3 is used for rectifying the second residue to obtain ethanol at the tower top;
the ethanol separation tower top separator 9 is used for mixing and contacting the second distillate and water for extraction and separation to obtain a water phase and an oil phase;
and the ethyl acetate rectifying tower 4 is used for rectifying the oil phase to obtain a fourth distillate at the tower top and obtain ethyl acetate at the tower bottom.
According to a preferred embodiment of the invention, the device further comprises: a first condenser 7, the first condenser 7 is used for condensing the second distillate. The first condenser 7 may be installed on a communicating line between the outlet of the top of the ethanol separation column 2 and the inlet of the top separator 9 of the ethanol separation column.
According to a preferred embodiment of the present invention, the outlet of the ethanol separation column overhead separator 9 communicates with the inlet of the ethanol separation column 2, so that the aqueous phase is returned to the ethanol separation column 2. This preferred embodiment allows further separation of the ethanol from the aqueous phase.
According to the device provided by the invention, the oil phase obtained by the separator 9 at the top of the ethanol separation tower is rectified in the ethyl acetate rectifying tower 4 to separate the ethyl acetate in the oil phase (obtained at the bottom of the ethyl acetate rectifying tower 4).
According to a preferred embodiment of the present invention, the bottom outlet of the ethanol rectification column 3 communicates with the inlet of the ethanol separation column overhead separator 9, so that the third residue is returned to the ethanol separation column overhead separator 9. With this preferred embodiment, the water in the system is fully utilized and the third residue is used to provide the water required in the overhead separator 9 of the ethanol separation column, reducing the use of fresh water.
According to the apparatus provided by the present invention, preferably, the apparatus further comprises: and a gas-liquid separator 11 for performing gas-liquid separation on the fourth distillate, wherein a gas phase mainly containing acetaldehyde is obtained at the top of the gas-liquid separator 11, and a liquid phase mainly containing ethyl acetate and ethanol is obtained at the bottom of the gas-liquid separator 11. By adopting the preferred embodiment, the product yield is more favorably improved.
According to an embodiment of the invention, the apparatus further comprises: a second condenser 8, the second condenser 8 is used for condensing the fourth distillate. The second condenser 8 may be installed on a communicating pipe between an outlet of the top of the ethyl acetate rectification column 4 and an inlet of the gas-liquid separator 11.
According to the apparatus provided by the present invention, preferably, the bottom of the gas-liquid separator 11 is connected to the inlet of the ethanol separation column overhead separator 9 so that the liquid phase containing ethyl acetate and ethanol is returned to the ethanol separation column overhead separator 9. The preferred embodiment can further separate and utilize ethyl acetate and ethanol in the solution.
According to a preferred embodiment of the present invention, the ethyl acetate rectification column 4 has a side draw, and a side stream is obtained from the side draw of the ethyl acetate rectification column 4; further preferably, a side line outlet of the ethyl acetate rectifying tower 4 is communicated with a side line separator 10, and the side line separator 10 is used for mixing and contacting the side stream with water for extraction and separation to obtain a water phase (discharged) and an oil phase; more preferably, the outlet of the side line separator 10 is communicated with the inlet of the ethyl acetate rectification column 4, so that the oil phase obtained by extraction separation in the side line separator 10 is returned to the ethyl acetate rectification column 4. This preferred embodiment is more advantageous in increasing the yield of ethyl acetate.
According to a preferred embodiment of the invention, the device further comprises: the acetic acid separation tower 1 is used for distilling and separating the materials to be separated to obtain a first distillate at the tower top and a first residue mainly containing acetic acid and water at the tower bottom; the overhead outlet of the acetic acid separation column 1 communicates with the inlet of the ethanol separation column 2, so that the first distillate is subjected to the distillation separation in the ethanol separation column 2. The skilled person will be able to select whether the plant is equipped with an acetic acid separation column 1 or not, depending on the specific composition of the material to be separated.
According to the invention, the material to be separated is preferably preheated and then sent to the acetic acid separation column 1 for distillation separation. In order to effectively utilize the heat source in the system, preferably, the apparatus further comprises: and the heat exchanger 5 is used for exchanging heat between the third residue obtained at the bottom of the ethanol rectifying tower 3 and the material to be separated. The heat exchanger 5 can be arranged on a communicating pipeline between the outlet at the bottom of the ethanol rectifying tower 3 and the inlet of the top separator 9 of the ethanol separation tower. This preferred embodiment enables preheating of the material to be separated by means of the heat of the third residue.
According to an embodiment of the invention, the apparatus further comprises: and a cooler 6 for cooling the third residue heat-exchanged by the heat exchanger 5 and then sending the third residue to a top separator 9 of the ethanol separation column. The cooler 6 may be installed on a line connecting the heat exchanger 5 and the inlet of the overhead separator 9 of the ethanol separation column.
According to a particular embodiment of the invention, the device comprises: the device comprises an ethanol separation tower 2, an ethanol rectifying tower 3, an ethanol separation tower top separator 9 and an ethyl acetate rectifying tower 4, wherein a tower top outlet of the ethanol separation tower 2 is communicated with an inlet of the ethanol separation tower top separator 9, a tower bottom outlet is communicated with an inlet of the ethanol rectifying tower 3, and an oil phase outlet of the ethanol separation tower top separator 9 is communicated with an inlet of the ethyl acetate rectifying tower 4. Preferably, the water phase outlet of the overhead separator 9 of the ethanol separation column is communicated with the inlet of the ethanol separation column 2.
The present invention will be described in detail below by way of examples.
Example 1
This example is provided to illustrate the method and apparatus for separating ethanol from ethyl acetate provided by the present invention.
1) As shown in figure 1, a material to be separated (the specific composition is shown in table 1) containing ethanol, ethyl acetate and acetic acid is preheated to 59 ℃ through a heat exchanger 5 and sent into an acetic acid separation tower 1 for distillation separation (the specific conditions are shown in table 2), a first distillate is obtained at the tower top, and a first residue mainly containing acetic acid and water is obtained at the tower bottom.
2) Feeding the first distillate into an ethanol separation tower 2 for distillation separation (the specific conditions are shown in table 2), obtaining a second distillate at the tower top, obtaining a second residue mainly containing ethanol and water at the tower bottom, rectifying the second residue in an ethanol rectifying tower 3 (the specific conditions are shown in table 2), obtaining ethanol at the tower top, and obtaining a third residue at the tower bottom.
3) A heat exchanger 5 and a cooler 6 are arranged on a communicating pipeline of the third residue and a top separator 9 of the ethanol separation tower, the heat exchanger 5 is used for exchanging heat between part of the third residue (the rest is discharged outside) and a material to be separated, the cooler 6 is used for cooling (cooling to 50 ℃) the part of the third residue after exchanging heat with the heat exchanger 5, and the part of the third residue after being cooled by the cooler 6 and a second distillate after being condensed to 25 ℃ by the first condenser 7 are sent to the top separator 9 of the ethanol separation tower for extraction and separation (specific conditions: temperature 25 deg.c and pressure 0.08MPa) to obtain an aqueous phase and an oil phase, wherein the mass ratio of the portion of the third residue, calculated as water, to the second distillate, calculated as ethanol, is 2.8: 1. The aqueous phase is returned to the ethanol separation column 2.
4) And (3) feeding the oil phase into an ethyl acetate rectifying tower 4 for rectification (the specific conditions are shown in table 2), so as to obtain a fourth distillate at the tower top and obtain ethyl acetate at the tower bottom.
5) Condensing the fourth distillate to 40 ℃ by a second condenser 8, and then sending the fourth distillate into a gas-liquid separator 11 for gas-liquid separation (the temperature is 40 ℃) so that a gas phase mainly containing acetaldehyde is obtained at the top of the gas-liquid separator 11, and a liquid phase mainly containing ethyl acetate and ethanol is obtained at the bottom of the gas-liquid separator 11; the liquid phase, which contains mainly ethyl acetate and ethanol, is returned to the overhead separator 9 of the ethanol separation column.
6) The ethyl acetate rectification column 4 has a side draw outlet at the middle-upper part of the column (the draw temperature is 55 ℃, and the pressure is 0.06MPa), a side stream is obtained from the side draw outlet of the ethyl acetate rectification column 4, and the side stream and fresh water (the mass ratio of water to the side stream in terms of ethanol is 13.8:1) are sent to a side separator 10 for extraction separation (specific conditions: the temperature is 35 ℃), obtaining a water phase and an oil phase, returning the oil phase to the ethyl acetate rectifying tower 4, and discharging the water phase.
The distillate and residue compositions for each column in the above scheme are shown in Table 3.
TABLE 1 compositions of materials to be separated
TABLE 2 operating conditions of the columns
Note: in the tables, the temperature is in units of "° c" and the pressure is in units of "MPa".
TABLE 3 distillate and residue compositions for each column
Note: the composition of each component in each column is expressed in units of "% by weight" in the table.
As can be seen from the data in Table 3, the ethanol content in the overhead product (ethanol product) of the ethanol rectification column 3 is 95 wt%, and the ethyl acetate content in the bottom residue (ethyl acetate product) of the ethyl acetate rectification column 4 is 99.07 wt%.
Example 2
The raw material to be separated (see table 4 for specific composition) contained no acetic acid, and the apparatus did not include the acetic acid separation column 1. Specifically, the method comprises the following steps:
1) preheating a material to be separated containing ethanol and ethyl acetate to 54 ℃ by a heat exchanger 5, sending the material to an ethanol separation tower 2 for distillation separation (the specific conditions are shown in table 5), obtaining a second distillate at the tower top, obtaining a second residue mainly containing ethanol and water at the tower bottom, rectifying the second residue in an ethanol rectifying tower 3 (the specific conditions are shown in table 5), obtaining ethanol at the tower top, and obtaining a third residue at the tower bottom.
2) A heat exchanger 5 and a cooler 6 are arranged on a communicating pipeline of the third residue and a top separator 9 of the ethanol separation tower, the heat exchanger 5 is used for exchanging heat between part of the third residue (the rest is discharged outside) and a material to be separated, the cooler 6 is used for cooling (cooling to 50 ℃) the part of the third residue after exchanging heat with the heat exchanger 5, and the part of the third residue after being cooled by the cooler 6 and a second distillate after being condensed to 25 ℃ by the first condenser 7 are sent to the top separator 9 of the ethanol separation tower for extraction and separation (specific conditions: temperature 25 deg.c and pressure 0.08MPa) to obtain an aqueous phase and an oil phase, wherein the mass ratio of the portion of the third residue, calculated as water, to the second distillate, calculated as ethanol, is 17.5: 1. The aqueous phase is returned to the ethanol separation column 2.
3) And (3) feeding the oil phase into an ethyl acetate rectifying tower 4 for rectification (the specific conditions are shown in table 5), so as to obtain a fourth distillate at the tower top and obtain ethyl acetate at the tower bottom.
4) Condensing the fourth distillate to 40 ℃ by a second condenser 8, and then sending the fourth distillate into a gas-liquid separator 11 for gas-liquid separation (the temperature is 40 ℃) so that a gas phase mainly containing acetaldehyde is obtained at the top of the gas-liquid separator 11, and a liquid phase mainly containing ethyl acetate and ethanol is obtained at the bottom of the gas-liquid separator 11; the liquid phase, which contains mainly ethyl acetate and ethanol, is returned to the overhead separator 9 of the ethanol separation column.
5) The ethyl acetate rectification column 4 has a side draw outlet at the middle-upper part of the column (the draw temperature is 58 ℃, and the pressure is 0.08MPa), a side stream is obtained from the side draw outlet of the ethyl acetate rectification column 4, and the side stream and fresh water (the mass ratio of water to the side stream in terms of ethanol is 13.4:1) are sent to a side separator 10 for extraction separation (specific conditions: the temperature is 35 ℃), obtaining a water phase and an oil phase, returning the oil phase to the ethyl acetate rectifying tower 4, and discharging the water phase.
The distillate and residue compositions for each column in the above scheme are shown in Table 6.
TABLE 4 composition of materials to be separated
| Components | By weight% |
| Ethanol | 65.95 |
| Ethyl acetate | 4.52 |
| Acetaldehyde | 0.79 |
| N-propanol | 0.17 |
| Acetone (II) | 0.05 |
| Water (W) | 28.52 |
TABLE 5 operating conditions for the columns
Note: in the tables, the temperature is in units of "° c" and the pressure is in units of "MPa".
TABLE 6 distillate and residue compositions for each column
Note: the composition of each component in each column is expressed in units of "% by weight" in the table.
As can be seen from the data in Table 6, the ethanol content in the overhead product (ethanol product) of the ethanol rectification column 3 is 95.18 wt%, and the ethyl acetate content in the bottom residue (ethyl acetate product) of the ethyl acetate rectification column 4 is 99 wt%, so that the method and the device provided by the invention can separate ethanol from ethyl acetate sufficiently.
Example 3
The procedure is as in example 1, except that the specific composition of the feed to be separated is shown in Table 7 and the operating conditions of the columns are shown in Table 8; the mass ratio of a part of the third residue as water to the second distillate as ethanol in the overhead separator 9 of the ethanol separation column was 4.8:1, and the mass ratio of water to the side stream as ethanol in the side separator 10 was 12.1: 1. The distillate and residue compositions of each column are shown in table 9.
TABLE 7 compositions of materials to be separated
| Components | By weight% |
| Acetic Acid (AA) | 19.07 |
| Ethanol | 46.78 |
| Ethyl acetate | 8.72 |
| Acetaldehyde | 2.13 |
| N-propanol | 0.35 |
| Acetone (II) | 0.07 |
| Water (W) | 22.88 |
TABLE 8 operating conditions for the columns
Note: in the tables, the temperature is in units of "° c" and the pressure is in units of "MPa".
TABLE 9 distillate and residue compositions for each column
Note: the composition of each component in each column is expressed in units of "% by weight" in the table.
As can be seen from the data in Table 9, the ethanol content in the overhead product (ethanol product) of the ethanol rectification column 3 is 95.10 wt%, and the ethyl acetate content in the bottom residue (ethyl acetate product) of the ethyl acetate rectification column 4 is 99.01 wt%, so that the method and the device provided by the invention can separate ethanol from ethyl acetate sufficiently.
Comparative example 1
The process of example 1 is followed except that the plant does not comprise an ethanol separation column overhead separator 9 and the third residue is returned to the ethanol separation column 2, specifically:
1) same as example 1, step 1);
2) the same as in step 2) of example 1, except that the conditions for the distillation separation in the ethanol separation column 2 included: the temperature at the top of the tower is 62 ℃, the pressure at the top of the tower is 0.08MPa, the temperature at the bottom of the tower is 87 ℃, the pressure at the bottom of the tower is 0.12MPa, and the reflux ratio is 6;
3) as shown in fig. 2, a heat exchanger 5 and a cooler 6 are arranged on a communicating pipeline of the third residue and ethanol separation tower 2, the heat exchanger 5 is used for exchanging heat between part of the third residue (the rest part is discharged outside) and the material to be separated, the cooler 6 is used for cooling (cooling to 40 ℃) the part of the third residue which is exchanged heat by the heat exchanger 5, and then returning the part of the third residue to the ethanol separation tower 2, and the mass ratio of the part of the third residue calculated by water to the second distillate calculated by ethanol is 2.04: 1.
4) And (3) feeding the second distillate into an ethyl acetate rectifying tower 4 for rectification (the conditions are the same as those in example 1, except that the reflux ratio is 7), so that a fourth distillate is obtained at the tower top, and ethyl acetate is obtained at the tower bottom.
5) Condensing the fourth distillate to 40 ℃ by a second condenser 8, and then sending the fourth distillate into a gas-liquid separator 11 for gas-liquid separation (the specific conditions are the same as those in example 1), wherein a gas phase mainly containing acetaldehyde is obtained at the top of the gas-liquid separator 11, and a liquid phase mainly containing ethyl acetate and ethanol is obtained at the bottom of the gas-liquid separator 11; the liquid phase, which contains mainly ethyl acetate and ethanol, is returned to the ethanol separation column 2.
6) Same as example 1, step 6).
The distillate and residue compositions for each column in the above scheme are shown in Table 10.
TABLE 10 distillate and residue compositions for each column
As can be seen from the data in Table 10, the ethyl acetate concentration at the bottom of the ethyl acetate rectifying column 4 in example 1 was 99.07%, while that in the comparative example was only 72.9%, which did not meet the product purity requirement. In addition, comparative example 1 eliminates the overhead separator 9 of the ethanol separation column, and the third residue is directly introduced into the ethanol separation column 2 after passing through the heat exchanger 5, and although the mass ratio of water to ethanol in the third residue is decreased, since the ethanol and water of example 1 have been preliminarily separated, the amount of ethanol is decreased, and the total amount of the third residue to which water is mainly added is decreased as compared with comparative example 1.
Test example 1
The load of the ethanol separation column 2 in example 1 and comparative example 1 was calculated; and the concentration of ethyl acetate in the residue of the ethyl acetate rectification column 4 in example 1 and the concentration of ethyl acetate in the residue of the ethyl acetate rectification column 4 in comparative example 1 were measured; the results are shown in Table 11.
Wherein, the load of the top of the ethanol separation column 2 and the load of the bottom of the ethanol separation column are calculated by Aspen.
TABLE 11
As can be seen from Table 11 above, the process of the present invention has lower load at the top of the ethanol separation column than that of comparative example 1, and the ethyl acetate product has higher purity than that of comparative example 1. In conclusion, the method and the device provided by the invention can not only improve the purity of ethanol and ethyl acetate products, but also reduce energy consumption.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, numerous simple modifications can be made to the technical solution of the invention, including combinations of the individual specific technical features in any suitable way. The invention is not described in detail in order to avoid unnecessary repetition. These simple modifications and combinations should be considered as the disclosure of the present invention, and all fall within the scope of the present invention.
Claims (22)
1. A process for separating ethanol and ethyl acetate, the process comprising:
1) distilling and separating the material to be separated containing ethanol and ethyl acetate in an ethanol separation tower (2), obtaining a second distillate at the tower top, and obtaining a second residue mainly containing ethanol and water at the tower bottom; rectifying the second residue in an ethanol rectifying tower (3) to obtain ethanol at the tower top;
2) mixing and contacting the second distillate and water in a separator (9) at the top of the ethanol separation tower for extraction and separation to obtain a water phase and an oil phase;
3) rectifying the oil phase in an ethyl acetate rectifying tower (4) to obtain a fourth distillate at the tower top and ethyl acetate at the tower bottom;
wherein a third residue obtained at the bottom of the ethanol rectification column (3) is introduced into an ethanol separation column overhead separator (9) to provide the water;
wherein, in the materials to be separated, the content of ethanol is 45-70 wt%, the content of ethyl acetate is 1-20 wt%, the content of water is 10-35 wt%, the content of acetic acid is 0-20 wt%, the content of acetaldehyde is 0-3 wt%, and the total content of n-propanol and acetone is 0-2 wt%;
wherein, the conditions for distillation separation in the ethanol separation tower (2) comprise: the temperature at the top of the tower is 20-70 ℃, the pressure at the top of the tower is 0.01-0.1MPa, the temperature at the bottom of the tower is 60-88 ℃, the pressure at the bottom of the tower is 0.04-0.13MPa, the number of tower plates is 20-32, and the reflux ratio is 3-8;
wherein, the rectification conditions in the ethanol rectification tower (3) comprise: the temperature at the top of the tower is 30-78 ℃, the pressure at the top of the tower is 0.01-0.1MPa, the temperature at the bottom of the tower is 74-104 ℃, the pressure at the bottom of the tower is 0.04-0.13MPa, the number of tower plates is 29-40, and the reflux ratio is 10-20;
wherein, the rectification conditions in the ethyl acetate rectification tower (4) comprise: the temperature at the top of the tower is 47-64 ℃, the pressure at the top of the tower is 0.04-0.08MPa, the temperature at the bottom of the tower is 62-77 ℃, the pressure at the bottom of the tower is 0.06-0.1MPa, the number of tower plates is 18-26, and the reflux ratio is 3-8;
wherein, the conditions for extraction and separation in the overhead separator (9) of the ethanol separation tower comprise: the temperature is 20-30 ℃, and the pressure is 0.01-0.1 MPa.
2. The process according to claim 1, wherein the mass ratio of water to the second distillate in ethanol in step 2) is 2-18: 1.
3. The process according to claim 1, wherein the aqueous phase in step 2) is returned to the ethanol separation column (2).
4. The method of any of claims 1-3, wherein the method further comprises: and carrying out gas-liquid separation on the fourth distillate in a gas-liquid separator (11), wherein a gas phase mainly containing acetaldehyde is obtained at the top of the gas-liquid separator (11), and a liquid phase mainly containing ethyl acetate and ethanol is obtained at the bottom of the gas-liquid separator (11).
5. The method according to claim 4, wherein the conditions for gas-liquid separation in the gas-liquid separator (11) include: the temperature is 40-50 deg.C, and the pressure is 0.04-0.08 MPa.
6. A process according to claim 4, wherein the liquid phase, mainly comprising ethyl acetate and ethanol, is returned to the ethanol separation column overhead separator (9).
7. The method of claim 1, wherein the method further comprises: a side stream is taken from the side of the ethyl acetate rectifying tower (4).
8. The process of claim 7, wherein the withdrawal temperature is from 51 to 66 ℃ and the pressure is from 0.05 to 0.09 MPa.
9. The method as claimed in claim 7, wherein the side stream and water are contacted in a side separator (10) for extractive separation to obtain an aqueous phase and an oil phase.
10. A method according to claim 9, wherein the oil phase separated in the side line separator (10) is returned to the ethyl acetate rectification column (4).
11. The process as claimed in claim 10, wherein the mass ratio of water added in the side-line separator (10) to the side stream, calculated as ethanol, is from 5 to 20: 1.
12. The process as claimed in claim 11, wherein the mass ratio of water added in the side-line separator (10) to the side stream, calculated as ethanol, is from 10 to 15: 1.
13. The method of claim 1, wherein the material to be separated further comprises acetic acid, the method further comprising: the material to be separated is subjected to distillation separation in an acetic acid separation tower (1), a first distillate is obtained at the tower top, a first residue mainly containing acetic acid and water is obtained at the tower bottom, and the first distillate is subjected to the distillation separation in an ethanol separation tower (2).
14. The method according to claim 13, wherein the conditions for the distillation separation in the acetic acid separation column (1) include: the temperature at the top of the tower is 35-90 ℃, the pressure at the top of the tower is 0.01-0.11MPa, the temperature at the bottom of the tower is 97-130 ℃, the pressure at the bottom of the tower is 0.06-0.16MPa, the number of tower plates is 16-27, and the reflux ratio is 2.5-5.
15. An apparatus for separating ethanol and ethyl acetate, the apparatus comprising:
the ethanol separation tower (2) is used for distilling and separating the materials to be separated containing ethanol and ethyl acetate to obtain a second distillate at the tower top and a second residue mainly containing ethanol and water at the tower bottom;
the ethanol rectifying tower (3) is used for rectifying the second residue to obtain ethanol at the tower top and obtain a third residue at the tower bottom;
an ethanol separation tower top separator (9) for mixing and contacting the second distillate and water for extraction and separation to obtain a water phase and an oil phase;
the ethyl acetate rectifying tower (4) is used for rectifying the oil phase to obtain a fourth distillate at the tower top and ethyl acetate at the tower bottom;
wherein the top outlet of the ethanol separation tower (2) is communicated with the inlet of a top separator (9) of the ethanol separation tower, the bottom outlet of the ethanol separation tower is communicated with the inlet of an ethanol rectifying tower (3), and the oil phase outlet of the top separator (9) of the ethanol separation tower is communicated with the inlet of an ethyl acetate rectifying tower (4);
wherein the tower bottom outlet of the ethanol rectifying tower (3) is communicated with the inlet of the ethanol separating tower top separator (9), so that the third residue is returned to the ethanol separating tower top separator (9).
16. An apparatus according to claim 15, wherein the outlet of the ethanol separation column overhead separator (9) is in communication with the inlet of the ethanol separation column (2) such that the aqueous phase is returned to the ethanol separation column (2).
17. The apparatus of claim 15, wherein the apparatus further comprises: and the gas-liquid separator (11) is used for carrying out gas-liquid separation on the fourth distillate, wherein the top of the gas-liquid separator (11) obtains a gas phase mainly containing acetaldehyde, and the bottom of the gas-liquid separator (11) obtains a liquid phase mainly containing ethyl acetate and ethanol.
18. The apparatus according to claim 17, wherein the bottom of the gas-liquid separator (11) is connected to an inlet of the ethanol separation column overhead separator (9) such that the liquid phase containing ethyl acetate and ethanol is returned to the ethanol separation column overhead separator (9).
19. The apparatus of claim 15, wherein the ethyl acetate rectification column (4) has a side draw from which a side stream is obtained from the side draw of the ethyl acetate rectification column (4).
20. The device as claimed in claim 19, wherein a side draw outlet of the ethyl acetate rectifying tower (4) is communicated with a side line separator (10), and the side line separator (10) is used for carrying out extraction separation by mixing and contacting the side stream with water to obtain a water phase and an oil phase.
21. An apparatus as claimed in claim 20, wherein the outlet of the side line separator (10) is in communication with the inlet of the ethyl acetate rectification column (4) such that the oil phase extracted and separated in the side line separator (10) is returned to the ethyl acetate rectification column (4).
22. The apparatus of any one of claims 15-21, wherein the apparatus further comprises: the acetic acid separation tower (1) is used for distilling and separating materials to be separated to obtain a first distillate at the tower top and a first residue mainly containing acetic acid and water at the tower bottom;
the top outlet of the acetic acid separation tower (1) is communicated with the inlet of the ethanol separation tower (2), so that the first distillate is subjected to distillation separation in the ethanol separation tower (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811033769.8A CN110878006B (en) | 2018-09-05 | 2018-09-05 | Method and device for separating ethanol and ethyl acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811033769.8A CN110878006B (en) | 2018-09-05 | 2018-09-05 | Method and device for separating ethanol and ethyl acetate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110878006A CN110878006A (en) | 2020-03-13 |
| CN110878006B true CN110878006B (en) | 2022-05-13 |
Family
ID=69727672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811033769.8A Active CN110878006B (en) | 2018-09-05 | 2018-09-05 | Method and device for separating ethanol and ethyl acetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110878006B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112125802B (en) * | 2020-09-29 | 2021-07-09 | 中国石油大学胜利学院 | Extractive distillation separation system and method for ethyl acetate-isopropanol-water mixture |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1351988A (en) * | 2000-11-15 | 2002-06-05 | 中国科学院大连化学物理研究所 | Process for producing ethyl-acetate from synthetic gas through ethanol and acetic acid |
| CN102414149A (en) * | 2010-02-02 | 2012-04-11 | 国际人造丝公司 | Hydrolysis of ethyl acetate in ethanol separation process |
| WO2013019237A1 (en) * | 2011-08-03 | 2013-02-07 | Celanese International Corporation | Reducing acetals and/or esters during ethanol separation process |
| TW201309629A (en) * | 2011-08-03 | 2013-03-01 | Celanese Int Corp | Process for producing anhydrous ethanol using extractive distillation column |
| CN103038199A (en) * | 2010-07-09 | 2013-04-10 | 国际人造丝公司 | Separation of vapor crude alcohol product |
| CN103097326A (en) * | 2011-04-26 | 2013-05-08 | 国际人造丝公司 | Esterification of vapor crude product in the production of alcohols |
| CN105198704A (en) * | 2014-05-29 | 2015-12-30 | 中国石油化工股份有限公司 | Method for low-energy consumption acetic acid hydrogenation production of ethanol |
| CN105859521A (en) * | 2016-04-07 | 2016-08-17 | 上海华谊（集团）公司 | Method for recovering ethanol by hydrolysis of ethyl acetate |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9126125B2 (en) * | 2010-07-09 | 2015-09-08 | Celanese International Corporation | Reduced energy alcohol separation process having water removal |
| US8877987B2 (en) * | 2011-08-03 | 2014-11-04 | Celanese International Corportation | Process for producing anhydrous ethanol using extractive distillation column |
-
2018
- 2018-09-05 CN CN201811033769.8A patent/CN110878006B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1351988A (en) * | 2000-11-15 | 2002-06-05 | 中国科学院大连化学物理研究所 | Process for producing ethyl-acetate from synthetic gas through ethanol and acetic acid |
| CN102414149A (en) * | 2010-02-02 | 2012-04-11 | 国际人造丝公司 | Hydrolysis of ethyl acetate in ethanol separation process |
| CN103038199A (en) * | 2010-07-09 | 2013-04-10 | 国际人造丝公司 | Separation of vapor crude alcohol product |
| CN103097326A (en) * | 2011-04-26 | 2013-05-08 | 国际人造丝公司 | Esterification of vapor crude product in the production of alcohols |
| WO2013019237A1 (en) * | 2011-08-03 | 2013-02-07 | Celanese International Corporation | Reducing acetals and/or esters during ethanol separation process |
| TW201309629A (en) * | 2011-08-03 | 2013-03-01 | Celanese Int Corp | Process for producing anhydrous ethanol using extractive distillation column |
| CN105198704A (en) * | 2014-05-29 | 2015-12-30 | 中国石油化工股份有限公司 | Method for low-energy consumption acetic acid hydrogenation production of ethanol |
| CN105859521A (en) * | 2016-04-07 | 2016-08-17 | 上海华谊（集团）公司 | Method for recovering ethanol by hydrolysis of ethyl acetate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110878006A (en) | 2020-03-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9169186B2 (en) | System and method for continuously producing polyoxymethylene dimethyl ethers | |
| CN111377800B (en) | Separation device and separation method for coal-to-ethanol liquid phase product | |
| CN108558603B (en) | Three-tower three-effect crude methanol refining process method | |
| CN110862301B (en) | Sec-butyl alcohol refining method and device | |
| CN111377802B (en) | Preparation method and system of sec-butyl alcohol | |
| CN105111079A (en) | Method and device for separating acetic acid sec-butyl ester and sec-butyl alcohol | |
| CN108002995B (en) | Method and equipment for synthesizing methyl isobutyl ketone by acetone two-step method | |
| CN101412665B (en) | Apparatus for coproduction of refined methanol and dimethyl ether or production of each of refined methanol and dimethyl ether from coarse methyl alcohol | |
| WO2020015321A1 (en) | Method and device for separating isopropanol | |
| CN103274913A (en) | Method and device for producing methyl isobutyl ketone | |
| CN111072481A (en) | Device and method for producing high-concentration dimethyl carbonate | |
| CN105669379A (en) | Technology for preparing ethanol from acetic ether through hydrogenation | |
| CN111170863A (en) | Energy-saving process method and device for purifying dimethyl carbonate by adopting four-tower heat integration | |
| CN110878006B (en) | Method and device for separating ethanol and ethyl acetate | |
| CN111100004A (en) | Method and integrated device for refining dimethyl carbonate | |
| CN107141213A (en) | A kind of method of acetic acid synthesis from methanol carbonylation | |
| CN111377801B (en) | Method and system for refining low carbon alcohol | |
| WO2021227136A1 (en) | Enhanced reaction system and method for preparing cyclohexanone by selective hydrogenation of benzene | |
| CN106518675A (en) | Dimethyl oxalate production method with byproduct (dimethyl carbonate) | |
| CN212199065U (en) | Separation device for coal-to-ethanol liquid-phase product | |
| CN112479869B (en) | Method for rectifying dimethyl oxalate in coal chemical industry | |
| CN211814215U (en) | Device for producing high-concentration dimethyl carbonate | |
| CN111285755B (en) | Separation method of reaction product for preparing dimethyl ether by methanol dehydration | |
| CN216725835U (en) | Partition plate type methyl propionate reaction rectifying tower with coupling hydrogenation | |
| CN110668920A (en) | Method for preparing ethanol and co-producing cyclohexanol by using reactive distillation method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 100011 Beijing Dongcheng District, West Binhe Road, No. 22 Applicant after: CHINA ENERGY INVESTMENT Corp.,Ltd. Applicant after: Beijing low carbon clean energy research institute Address before: 100011 Beijing Dongcheng District, West Binhe Road, No. 22 Applicant before: CHINA ENERGY INVESTMENT Corp.,Ltd. Applicant before: Beijing low carbon clean energy research institute |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |