CN112778087A - Method for separating methanol-toluene azeotrope through continuous extractive distillation - Google Patents
Method for separating methanol-toluene azeotrope through continuous extractive distillation Download PDFInfo
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- CN112778087A CN112778087A CN202110027800.2A CN202110027800A CN112778087A CN 112778087 A CN112778087 A CN 112778087A CN 202110027800 A CN202110027800 A CN 202110027800A CN 112778087 A CN112778087 A CN 112778087A
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- 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
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
Abstract
The invention discloses a method for separating a methanol-toluene azeotrope by continuous extractive distillation. The method uses butyl butyrate as an extracting agent, adopts a continuous extraction rectification method to separate a methanol-toluene azeotropic mixture, methanol and toluene are mixed and fed, the reflux ratio is 0.5-1.5, the molar flow ratio of the extracting agent to raw materials is 0.5-2, the top fraction of an extraction rectification tower is a methanol product, the bottom fraction of the tower is a mixture of toluene and the extracting agent, the discharged material at the bottom of the tower enters a solvent recovery tower, toluene is obtained at the top of the solvent recovery tower, the extracting agent is obtained at the bottom of the tower, and the extracting agent can be recycled. The method has the advantages of simple process, low cost, easy operation, high continuous rectification efficiency and simple solvent recovery, and the mole fraction of the treated methanol and toluene products is not less than 0.999, and can be applied to industrialization.
Description
Technical Field
The invention belongs to the technical field of chemical separation, and particularly relates to a method for separating a methanol-toluene azeotrope by continuous extractive distillation.
Background
Methanol is one of the basic organic raw materials, and is used for manufacturing various organic products such as methyl chloride, methylamine, dimethyl sulfate and the like. Also is a raw material for pesticides (insecticides, acaricides) and medicines (sulfonamides, synbiotics, etc.), and is one of raw materials for synthesizing dimethyl terephthalate, methyl methacrylate and methyl acrylate.
Toluene is produced from crude oil by petrochemical processes. It is used as solvent for oil, resin, natural rubber and synthetic rubber, coal tar, asphalt, cellulose acetate, as solvent for cellulose paint and varnish, and as solvent for photo-plate and ink. Toluene is also a raw material for organic synthesis, particularly benzoyl chloride and organic synthesis of phenyl, saccharin, trinitrotoluene and many dyes. It is also a component of aviation and automotive gasoline. However, under the normal atmospheric pressure, methanol and toluene form a minimum azeotropic mixture, the azeotropic molar compositions of the methanol and the toluene are respectively 88.2 percent and 11.8 percent, and the methanol and the toluene are difficult to separate by ordinary rectification.
The literature (Yangming, Depeng, leaf dreaming, high-new. research on the process of separating methanol-toluene by coupling extraction-rectification with salt [ J ]. chemical engineering, 2014,42(05):31-34.) proposes a 3-column process flow of separating methanol-toluene by coupling extraction-rectification with salt, when the number of theoretical plates of the extraction column is 5; the theoretical plate number of the methanol recovery tower is 21, and the reflux ratio is 1.8; when the theoretical plate number of the toluene recovery tower is 28 and the reflux ratio is 2.4, the mass fractions of the methanol and the toluene obtained by separation are 0.996 and 0.997 respectively. The salt corrosion-prone equipment has high requirements on equipment materials, and is difficult to be applied industrially or produced in large quantities.
According to the literature (Ting, Levensiu. simulation of extractive distillation separation of a toluene-methanol azeotropic system [ J ]. Shandong chemical engineering 2020,49(02): 152-. Based on AspenPlus process simulation software, the process simulation is carried out on the extraction rectification process of the toluene-methanol mixture, and the optimal process parameters of the extraction rectification tower are determined, wherein the solvent ratio is 0.6, the number of theoretical plates of the whole tower is 38, the feeding positions of ionic liquid and raw materials are respectively a No. 2 tower plate and a No. 27 tower plate, and the reflux ratio is 2.2. Under the condition, toluene with a molar fraction of 99.9% can be obtained at the top of the column. The ionic liquid has high cost, high viscosity and easy corrosion to equipment, and is difficult to be applied industrially or produced in large quantities.
According to the literature (simulation research on extraction and rectification processes of pigments, Luoxian, Zhangjuan, Wankelang, phyllun, methanol-toluene azeotrope [ J ] scientific wind, 2017(25):137 +143 + 138-), cyclohexanol is selected as an extracting agent, and the optimal process parameters of an extraction and rectification tower and an extracting agent regeneration tower are determined, wherein under the process conditions, the mole fraction of methanol reaches 99.8%, and the mole fraction of toluene also reaches 99.8%. However, cyclohexanol has moderate toxicity, high toxicity, easy crystallization at low temperature, high viscosity and poor flowability.
According to the research on the separation of a methanol-toluene azeotrope by extractive distillation [ J ] in chemical industry and engineering, 2013,30(05):71-75.) in the literature (happily luan, Zhang Jinwei, Zhuhongji, Baipeng, Li Bo, Sun Chang.) the methanol product with the mole fraction of 99.688% is obtained at the top of a tower under the operation of batch extractive distillation tower with the tower plate number of 30, the solvent ratio of 1 and the constant reflux ratio (R ═ 3). But o-xylene has anesthetic property, high toxicity and potential safety hazard.
In the literature (Li Y, Xu C. Pressure-Swing Distillation for Separating Pressure-sensitive Methanol/Toluene, minor constituent minim hydrogenation azo-catalyst/Toluene via intrinsic Light Entrainer: Design and Control [ J ]. Industrial & Engineering Chemistry Research,2017,56(14): 4017-. However, chloroform is low toxic, anesthetic and carcinogenic.
The patent (201510753892.7) discloses a method for separating a mixed solution of methanol and toluene by combining external circulation extractive distillation and internal condensation layering. The purity of the methanol obtained by the application embodiment is 99.10 percent, and the purity of the toluene is 99.00 percent. The method adopts intermittent extraction and rectification, and is not suitable for continuous production.
The rectification industry has been developing for decades and mainly includes extractive rectification, azeotropic rectification, salt-added rectification, pressure swing rectification, molecular rectification, etc. The design can realize the destruction of a methanol-toluene azeotropic system by an extraction rectification process and an organic solvent extractant, and two high-purity products are obtained.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides the method for separating the methanol and toluene azeotrope, which has high product purity and simple operation.
The invention is realized by the following technical scheme:
a method for separating an azeotropic mixture of methanol and toluene by extractive distillation is characterized in that the device used by the method comprises the following components:
an extractive distillation tower (T1), a condenser (C1), a reflux tank (R1), a reboiler (B1), a solvent recovery tower (T2), a condenser (C2), a reflux tank (R2) and a reboiler (B2); wherein the condenser (C1) is connected to the top of the extractive distillation column (T1), the reflux tank (R1) is connected to the condenser (C1), the reboiler (B1) is connected to the bottom of the extractive distillation column (T1), the condenser (C2) is connected to the top of the solvent recovery column (T2), the reflux tank (R2) is connected to the condenser (C2), and the reboiler (B2) is connected to the bottom of the solvent recovery column (T2);
the method mainly comprises the following steps:
(1) a mixture of methanol and toluene enters from the middle lower part of an extractive distillation tower (T1) through a raw material liquid feed pump (P1), an extractant enters from the upper part of the extractive distillation tower (T1) through an extractant feed pump (P2), the overhead stream of the extractive distillation tower (T1) is condensed through a condenser (C1), and after being stored in a reflux tank (R1), one part of the overhead stream is extracted as a product, and the other part of the overhead stream reflows to the extractive distillation tower (T1);
(2) the bottom stream of the extractive distillation column (T1) is a feed stream of a solvent recovery column (T2), enters the solvent recovery column (T2) through a feed pump (P3) of the solvent recovery column, and is separated from the toluene;
(3) after the overhead stream of the solvent recovery tower (T2) is condensed by a condenser (C2) and stored in a reflux tank (R2), one part of the overhead stream is extracted as a product, and the other part of the overhead stream is refluxed to the solvent recovery tower (T2);
(4) the bottom material of the solvent recovery tower (T2) flows through an extractant circulating pump (P4) and enters a condenser (C3), and the condensed bottom material is mixed with an extractant S flow for recycling;
the patent proposes a more preferred process in which the number of theoretical plates of the extractive rectification column (T1) is from 40 to 55, the feed position of the mixture is from 28 to 42, and the feed position of the extractant is from 5 to 15; the number of trays in the solvent recovery column (T2) is 20 to 35, and the feed position is 12 to 26.
This patent proposes a more preferred process in which the ratio of the molar flow of extractant to feedstock is in the range 0.5 to 2.
This patent proposes a more preferred process in which the methanol and toluene are azeotropes, the mole fraction of methanol being in the range of 0.2 to 0.6 and the mole fraction of toluene being in the range of 0.4 to 0.8.
Compared with the prior art, the invention mainly has the following gain effects:
(1) the method adopts extractive distillation operation, and has the advantages of simple operation and high product purity;
(2) the recovery rate of the extracting agent is high, the extracting agent can be recycled, the cost is reduced, and the pollution to the environment is reduced.
Drawings
FIG. 1 is a flow chart of the process for separating a mixture of methanol and toluene by extractive distillation according to the present invention.
T1-extractive distillation column; t2-solvent recovery column; c1, C2-overhead condenser; c3-condenser; b1, B2-bottom reboiler; r1, R2-reflux drum; p1, P2, P3, P4-pump.
Detailed Description
The present invention will be described in terms of the following examples, which illustrate the effect of separating a mixture of methanol and toluene by extractive distillation using butyl butyrate as an extractant, but the present invention is not limited to the following examples, and various examples are included in the technical scope of the present invention within the scope not departing from the spirit of the invention described above and below.
Example 1
The extractive distillation flow path is shown in figure 1. The number of theoretical plates of extractive distillation column T1 was 50, extractant butyl butyrate S was fed from plate 8 at a flow rate of 100kmol/h, and mixture of methanol and toluene (methanol 0.5+ toluene 0.5) F was fed from plate 30 at a flow rate of 100 kmol/h. The extractive distillation tower T1 is operated under normal pressure, the reflux ratio is 0.8, the extraction amount at the tower top is 49.985kmol/h, a methanol product with the mole fraction of 0.999 is obtained at the tower top, a mixture W of toluene and an extractant butyl butyrate is obtained at the tower bottom, the mixture W enters a solvent recovery tower T2 from the 18 th tower plate, the theoretical number of the tower plates of the solvent recovery tower T2 is 30, the reflux ratio is 1.2, the extraction amount at the tower top is 49.96kmol/h, the toluene with the mole fraction of 0.999 is obtained at the tower top, the extractant butyl butyrate with the mole fraction of 0.9999 is obtained at the tower bottom, and the condensed extractant butyl butyrate is mixed with an extractant S stream for recycling.
Example 2
The extractive distillation flow path is shown in figure 1. The number of theoretical plates of extractive rectification column T1 was 46, the extractant butyl butyrate S was fed from the 10 th plate at a flow rate of 80kmol/h, and the mixture of methanol and toluene (methanol 0.2+ toluene 0.8) F was fed from the 32 th plate at a flow rate of 100 kmol/h. The extractive distillation tower T1 is operated under normal pressure, the reflux ratio is 0.6, the extraction amount at the tower top is 20.739kmol/h, a methanol product with the mole fraction of 0.999 is obtained at the tower top, a mixture W of toluene and an extractant butyl butyrate is obtained at the tower bottom, the mixture W enters a solvent recovery tower T2 from the 12 th tower plate, the theoretical number of the tower plates of the solvent recovery tower T2 is 28, the reflux ratio is 0.95, the extraction amount at the tower top is 79.228kmol/h, the toluene with the mole fraction of 0.999 is obtained at the tower top, the extractant butyl butyrate with the mole fraction of 0.9999 is obtained at the tower bottom, and the condensed extractant butyl butyrate is mixed with an extractant S stream for recycling.
Example 3
The extractive distillation flow path is shown in figure 1. The number of theoretical plates of extractive rectification column T1 was 52, the extractant butyl butyrate S was fed from the 12 th plate at a flow rate of 115kmol/h, and the mixture of methanol and toluene (methanol 0.35+ toluene 0.65) F was fed from the 38 th plate at a flow rate of 100 kmol/h. The extractive distillation tower T1 is operated under normal pressure, the reflux ratio is 1.25, the overhead output is 34.96kmol/h, a methanol product with the mole fraction of 0.999 is obtained at the tower top, a mixture W of toluene and an extractant butyl butyrate is obtained at the tower bottom, the mixture W enters a solvent recovery tower T2 from the 18 th tower plate, the theoretical number of the tower plates of the solvent recovery tower T2 is 33, the reflux ratio is 1.6, the overhead output is 64.93kmol/h, the toluene with the mole fraction of 0.999 is obtained at the tower top, the extractant butyl butyrate with the mole fraction of 0.9999 is obtained at the tower bottom, and the condensed extractant butyl butyrate is mixed with an extractant S stream for recycling.
Example 4
The extractive distillation flow path is shown in figure 1. The number of theoretical plates of extractive rectification column T1 was 55, extractant butyl butyrate S was fed from the 15 th plate at a flow rate of 135kmol/h, and a mixture of methanol and toluene (methanol 0.6+ toluene 0.4) F was fed from the 38 th plate at a flow rate of 100 kmol/h. The extractive distillation tower T1 is operated under normal pressure, the reflux ratio is 1.33, the extraction amount at the tower top is 59.968kmol/h, a methanol product with the mole fraction of 0.999 is obtained at the tower top, a mixture W of toluene and an extractant butyl butyrate is obtained at the tower bottom, the mixture W enters a solvent recovery tower T2 from a 16 th tower plate, the theoretical tower plate number of the solvent recovery tower T2 is 32, the reflux ratio is 1.39, the extraction amount at the tower top is 39.947kmol/h, the toluene with the mole fraction of 0.999 is obtained at the tower top, the extractant butyl butyrate with the mole fraction of 0.9999 is obtained at the tower bottom, and the condensed extractant butyl butyrate is mixed with an extractant S stream for recycling.
Claims (4)
1. A method for separating methanol-toluene azeotrope by continuous extractive distillation is characterized in that an extractive distillation method using butyl butyrate as an extracting agent is adopted, and the used device comprises the following components:
an extractive distillation tower (T1), a condenser (C1), a reflux tank (R1), a reboiler (B1), a raw material liquid feed pump (P1), an extractant feed pump (P2), a solvent recovery tower (T2), a solvent recovery tower feed pump (P3), an extractant circulating pump (P4), a condenser (C2), a condenser (C3), a reflux tank (R2) and a reboiler (B2); wherein the condenser (C1) is connected to the top of the extractive distillation column (T1), the reflux tank (R1) is connected to the condenser (C1), the reboiler (B1) is connected to the bottom of the extractive distillation column (T1), the condenser (C2) is connected to the top of the solvent recovery column (T2), the reflux tank (R2) is connected to the condenser (C2), and the reboiler (B2) is connected to the bottom of the solvent recovery column (T2);
the method mainly comprises the following steps:
(1) a mixture of methanol and toluene enters from the middle lower part of an extractive distillation tower (T1) through a raw material liquid feed pump (P1), an extractant enters from the upper part of the extractive distillation tower (T1) through an extractant feed pump (P2), the overhead stream of the extractive distillation tower (T1) is condensed through a condenser (C1), and after being stored in a reflux tank (R1), one part of the overhead stream is extracted as a product, and the other part of the overhead stream reflows to the extractive distillation tower (T1);
(2) the bottom stream of the extractive distillation column (T1) is a feed stream of a solvent recovery column (T2), enters the solvent recovery column (T2) through a feed pump (P3) of the solvent recovery column, and is separated from the toluene;
(3) after the overhead stream of the solvent recovery tower (T2) is condensed by a condenser (C2) and stored in a reflux tank (R2), one part of the overhead stream is extracted as a product, and the other part of the overhead stream is refluxed to the solvent recovery tower (T2);
(4) the bottom material of the solvent recovery tower (T2) flows through an extractant circulating pump (P4) and enters a condenser (C3), and the condensed bottom material is mixed with an extractant S flow for recycling;
wherein the pressure of the extraction rectifying tower (T1) is 1atm, the reflux ratio is 0.5-1.5, the pressure of the solvent recovery tower (T2) is 1atm, and the reflux ratio is 0.7-2.2;
the temperature of the top of the extraction and rectification tower (T1) is 63-68 ℃, and the temperature of the bottom of the extraction and rectification tower is 130-160 ℃; the temperature at the top of the solvent recovery tower (T2) is 105 ℃ plus 118 ℃, and the temperature at the bottom of the solvent recovery tower is 165 ℃ plus 180 ℃;
the molar purity of the methanol and the toluene products separated by the method is more than 0.999, and the molar purity of the butyl butyrate serving as an extractant is more than 0.9999.
2. The process as claimed in claim 1, characterized in that the number of theoretical plates of the extractive distillation column (T1) is 40 to 55, the feed position of the mixture is 28 to 42, and the feed position of the extractant is 5 to 15; the number of trays in the solvent recovery column (T2) is 20 to 35, and the feed position is 12 to 26.
3. The process of claim 1, wherein the ratio of the molar flow rate of the extractant to the feed is 0.5 to 2.
4. The process of claim 1, wherein the methanol/toluene azeotrope has a methanol mole fraction of 0.2 to 0.6 and a toluene mole fraction of 0.4 to 0.8.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114163288A (en) * | 2021-12-01 | 2022-03-11 | 沈阳化工大学 | Method for separating toluene-methanol by extractive distillation |
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