CN111606877B - Acetic acid azeotropic dehydration device and method suitable for producing trimellitic anhydride - Google Patents
Acetic acid azeotropic dehydration device and method suitable for producing trimellitic anhydride Download PDFInfo
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- CN111606877B CN111606877B CN202010521034.0A CN202010521034A CN111606877B CN 111606877 B CN111606877 B CN 111606877B CN 202010521034 A CN202010521034 A CN 202010521034A CN 111606877 B CN111606877 B CN 111606877B
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/87—Benzo [c] furans; Hydrogenated benzo [c] furans
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- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
- B01D3/36—Azeotropic distillation
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Abstract
The invention provides an acetic acid azeotropic dehydration device suitable for producing trimellitic anhydride, which comprises an azeotropic distillation tower and a solvent recovery tower, wherein the azeotropic distillation tower is connected with a condenser I pipeline at the top of the azeotropic distillation tower, the condenser I is connected with an oil-water phase separation tank through a pipeline, an oil phase partition of the oil-water phase separation tank is connected with the azeotropic distillation tower pipeline through a distribution line V, a water phase partition is connected with a distribution line III, one outlet of the distribution line III is connected with the distribution line V pipeline, and the other outlet of the distribution line III is connected with the solvent recovery tower pipeline; the solvent recovery tower is connected with a liquid-liquid phase separation tank through a condenser II; the liquid-liquid phase-splitting tank is connected with the IPA middle storage tank and the middle storage tank pipeline respectively. The invention can continuously carry out azeotropic dehydration of acetic acid, and has small equipment investment and low production energy consumption.
Description
Technical Field
The invention relates to a trimellitic anhydride production device, in particular to a low-energy consumption water removal device for aqueous acetic acid in the trimellitic anhydride production process.
Background
Trimellitic anhydride, abbreviated as meta anhydride or TMA. The production process is to prepare trimellitic acid from trimellitic acid and then prepare trimellitic anhydride. The acetic acid azeotropic separation technology is mostly used for PTA devices, in the trimellitic anhydride production device, because the large-scale production cannot be realized, the total amount of the aqueous acetic acid is not large, and the acetic acid contains a small amount of trimellitic benzene, so that the trimellitic benzene is recovered, and the existing devices mostly adopt a thermal coupling tower to separate water and recover trimellitic anhydride. Because acetic acid is highly corrosive, the separation tower must be made of special materials. Generally, the method has the factors of large equipment investment, high energy consumption, and the like, which are unfavorable for reducing the production cost.
Disclosure of Invention
The technical problem to be solved by the invention is to provide the acetic acid azeotropic dehydration device suitable for producing trimellitic anhydride, which can continuously carry out acetic acid azeotropic dehydration, and has the advantages of low equipment investment and low production energy consumption.
In order to solve the technical problems, the acetic acid azeotropic dehydration device suitable for producing trimellitic anhydride comprises an azeotropic distillation tower and a solvent recovery tower, wherein a condenser I is arranged above the azeotropic distillation tower, the azeotropic distillation tower is connected with the condenser I through a pipeline at the top of the azeotropic distillation tower, and an acetic acid product storage tank is connected to the bottom of the azeotropic distillation tower; the condenser I is connected with an oil-water phase-splitting tank through a pipeline, an oil phase partition of the oil-water phase-splitting tank is connected with the azeotropic distillation tower through a distribution line V, and an oil phase distribution pump and a valve II are arranged on the distribution line V; the water phase partition of the oil-water phase separation tank is connected with a distribution line III through a water phase distribution pump, one outlet of the distribution line III is connected with a distribution line V through a valve III in a pipeline manner, and the other outlet of the distribution line III is connected with a solvent recovery tower through a valve IV in a pipeline manner; the top pipeline of the solvent recovery tower is connected with a condenser II, and the condenser II is connected with a liquid-liquid phase separation tank through a pipeline; an outlet of the liquid-liquid phase separation tank is connected with an IPA intermediate storage tank through a valve V, the IPA intermediate storage tank is connected with a distribution line I through a reflux distribution pump, and the distribution line I is connected with an oil phase partition pipeline of the oil-water phase separation tank through the valve I; and the other outlet of the liquid-liquid phase-splitting tank is connected with a PSC intermediate storage tank through a pipeline of a valve VI.
The liquid-liquid phase-splitting tank is arranged above the IPA middle storage tank and the PSC middle storage tank, so that the liquid after phase splitting by the liquid-liquid phase-splitting tank can flow into the two middle storage tanks respectively by self weight.
The invention also provides an acetic acid azeotropic dehydration method suitable for producing trimellitic anhydride, which comprises the following steps:
step 1: the azeotropic distillation dilute acetic acid raw material liquid with the concentration of 80-85 percent enters an azeotropic distillation tower after being preheated to 80+/-5 ℃, isopropyl acetate is simultaneously added into the tower to be used as an entrainer, the pressure in the tower kettle is controlled at 40-60 kpa, the temperature of the tower top is controlled at 52-60 ℃, and the temperature of the tower kettle is controlled at 100-110 ℃ through a reboiler so as to separate components with different boiling points.
Step 2: acetic acid with the concentration of 96% extracted from the bottom of the azeotropic distillation tower enters an acetic acid product storage tank, gas-phase dilute acetic acid, water and entrainer at the top of the azeotropic distillation tower are condensed by a condenser I and enter an oil-water phase separation tank for phase separation, an oil phase flows back into the azeotropic distillation tower by an oil phase distribution pump and a distribution line V, a water phase is output by the reflux distribution pump, part of the water phase is controlled to return into the top of the azeotropic distillation tower by a valve III, and the rest of the water phase enters a solvent recovery tower by a valve IV for re-separation;
step 3: the gas phase at the top of the solvent recovery tower is condensed by a condenser II and then enters a liquid-liquid phase-splitting tank, PSC and IPA are separated in the liquid-liquid phase-splitting tank after liquid-liquid phase splitting, the PSC and the IPA are respectively fed into a PSC intermediate storage tank and an IPA intermediate storage tank, and the recovery of the IPA intermediate storage tank is returned into the oil phase partition of the oil-water phase-splitting tank through a reflux distribution pump and a distribution line I.
In the step 2, the flow of the water phase returned from the oil-water phase separation tank to the top of the azeotropic distillation tower is equal to the flow of the oil phase through the control of a valve III.
The technical advantages of the invention are as follows: the isopropyl acetate is used as an entrainer to realize low-energy consumption continuous water removal of the aqueous acetic acid, so that the equipment investment is low and the production energy consumption is low.
Drawings
FIG. 1 is a schematic diagram of an azeotropic dehydration plant for acetic acid suitable for the production of trimellitic anhydride according to the invention.
Detailed Description
The following describes the embodiments of the present invention further with reference to the drawings.
As shown in fig. 1, the acetic acid azeotropic dehydration device suitable for producing trimellitic anhydride comprises an azeotropic distillation tower T1 and a solvent recovery tower T2, wherein a condenser IE 1 is arranged above the azeotropic distillation tower T1, the azeotropic distillation tower T1 is connected with the condenser IE 1 through a pipeline at the top part of the azeotropic distillation tower T1, and an acetic acid product storage tank is connected at the bottom part of the azeotropic distillation tower T1; the condenser IE 1 is connected with an oil-water phase-splitting tank D2 through a pipeline, an oil phase partition of the oil-water phase-splitting tank D2 is connected with the azeotropic distillation tower T1 through a distribution line VX 5, and the distribution line VX 5 is provided with an oil phase distribution pump P2 and a valve II V2; the water phase partition of the oil-water phase separation tank D2 is connected with a distribution line III X3 through a water phase distribution pump P3, one outlet of the distribution line III X3 is connected with a distribution line V X5 pipeline through a valve III V3, and the other outlet of the distribution line III X3 is connected with a solvent recovery tower T2 pipeline through a valve IV V4; the top pipeline of the solvent recovery tower T2 is connected with a condenser II E2, and the condenser II E2 is connected with a liquid-liquid phase separation tank D3 through a pipeline; an outlet of the liquid-liquid phase separation tank D3 is connected with an IPA intermediate storage tank D1 through a valve V5, the IPA intermediate storage tank D1 is connected with a distribution line IX 1 through a reflux distribution pump P1, and the distribution line IX 1 is connected with an oil phase partition pipeline of the oil-water phase separation tank D2 through a valve IV 1; the other outlet of the liquid-liquid phase-splitting tank D3 is connected with a PSC intermediate storage tank D4 through a valve VI V6 pipeline.
The liquid-liquid phase-splitting tank D3 is arranged above the IPA middle storage tank D1 and the PSC middle storage tank D4, so that the liquid separated by the liquid-liquid phase-splitting tank D3 can flow into the two middle storage tanks respectively under the dead weight.
The general idea of the invention is as follows: the aqueous acetic acid enters an azeotropic distillation tower, water is entrained to the top of the tower by IPA under the action of isopropyl acetate IPA, gas phase at the top of the tower enters an oil-water phase separation tank after being condensed, oil phase is returned to the top of the azeotropic distillation tower as reflux after being separated in the oil-water phase separation tank, water phase is partially used as reflux, and part of water phase is extracted from the oil-water phase separation tank as waste water to enter a solvent recovery tower T2, and acetic acid with qualified content is obtained at the bottom of the azeotropic distillation tower T1.
The water phase extracted from the oil-water phase separation tank D2 contains a small amount of IPA and PSC, the IPA and PSC extracted from the top of the solvent recovery tower T2 are separated again, the liquid phase separation is carried out by entering the liquid-liquid phase separation tank D3 from the top of the solvent recovery tower T2, PSC and IPA are separated for recycling, and wastewater at the bottom of the solvent recovery tower T2 is sent into a sewage treatment system.
The specific working procedure is as follows: an azeotropic dehydration method of acetic acid suitable for producing trimellitic anhydride, comprising the following steps:
step 1: the azeotropic distillation dilute acetic acid raw material liquid with the concentration of 80-85 percent enters an azeotropic distillation tower T1 after being preheated to 80+/-5 ℃, isopropyl acetate is added into the tower to be used as an entrainer, the pressure in the tower bottom is controlled at 40-60 kpa, the temperature of the tower top is controlled at 52-60 ℃, and the temperature of the tower bottom is controlled at 100-110 ℃ through a reboiler to separate components with different boiling points.
Step 2: acetic acid with the concentration of 96% extracted from the bottom of the azeotropic distillation tower T1 enters an acetic acid product storage tank, gas phase dilute acetic acid, water and entrainer at the top of the azeotropic distillation tower T1 are condensed by a condenser IE 1 and enter an oil-water phase separation tank D2 for phase separation, an oil phase flows back to enter the azeotropic distillation tower T1 by an oil phase distribution pump P2 and a distribution line VX 5, a water phase is output by a reflux distribution pump P3, part of the water phase is controlled to return to the top of the azeotropic distillation tower T1 by a valve IIIV 3, and the rest of the water phase enters a solvent recovery tower T2 by a valve IVV 4 for re-separation;
step 3: the gas phase at the top of the solvent recovery tower T2 is condensed by a condenser II E2 and then enters a liquid-liquid phase-splitting tank D3, PSC and IPA are separated in the liquid-liquid phase-splitting tank D3 after liquid-liquid phase splitting and respectively enter a PSC intermediate storage tank D4 and an IPA intermediate storage tank D1, and the recovery of the IPA intermediate storage tank D1 returns to the oil phase partition of the oil-water phase-splitting tank D2 through a reflux distribution pump P1 and a distribution line IX 1.
In the step 2, the flow of the water phase and the oil phase returned from the oil-water phase separation tank D2 to the top of the azeotropic distillation tower T1 are controlled by a valve III V3.
The invention realizes successful application in the production line of the I's maleic anhydride. Through actual operation, high-efficiency continuous operation is realized, equipment investment is effectively reduced, and energy consumption is reduced. Before transformation, a double-tower coupling operation mode is adopted, the investment of a single tower is about 600 ten thousand, the total investment is 1200 ten thousand yuan, and the total investment after the equipment is developed is about 900 ten thousand yuan; the acetic acid treatment capacity per unit hour before transformation is 10 tons, the steam consumption is about 12 tons, and the steam consumption of the azeotropic distillation tower after transformation is 8 tons/hour. Thus, the investment is reduced, and the continuous operation with low cost is realized.
The present invention is not limited to the above-described embodiments, and various modifications and variations can be made by those skilled in the art in light of the present invention without departing from the spirit and the essence of the invention, but still fall within the scope of the invention.
Claims (3)
1. Acetic acid azeotropic dehydration device suitable for producing trimellitic anhydride, including azeotropic distillation tower (T1), still include solvent recovery tower (T2), its characterized in that: a condenser I (E1) is arranged above the azeotropic distillation tower (T1), the top of the azeotropic distillation tower (T1) is connected with the condenser I (E1) through a pipeline, and the bottom of the azeotropic distillation tower (T1) is connected with an acetic acid product storage tank; the condenser I (E1) is connected with an oil-water phase-splitting tank (D2) through a pipeline, an oil phase partition of the oil-water phase-splitting tank (D2) is connected with the azeotropic distillation tower (T1) through a distribution line V (X5), and an oil phase distribution pump (P2) and a valve II (V2) are arranged on the distribution line V (X5); the water phase partition of the oil-water phase separation tank (D2) is connected with a distribution line III (X3) through a water phase distribution pump (P3), one outlet of the distribution line III (X3) is connected with a distribution line V (X5) through a valve III (V3) in a pipeline manner, and the other outlet of the distribution line III is connected with the solvent recovery tower (T2) through a valve IV (V4) in a pipeline manner; the top pipeline of the solvent recovery tower (T2) is connected with a condenser II (E2), and the condenser II (E2) is connected with a liquid-liquid phase separation tank (D3) through a pipeline; one outlet of the liquid-liquid phase separation tank (D3) is connected with an IPA intermediate storage tank (D1) through a valve V (V5), the IPA intermediate storage tank (D1) is connected with a distribution line I (X1) through a reflux distribution pump (P1), and the distribution line I (X1) is connected with an oil phase partition pipeline of the oil-water phase separation tank (D2) through the valve I (V1); the other outlet of the liquid-liquid phase-splitting tank (D3) is connected with a PSC intermediate storage tank (D4) through a valve VI (V6) pipeline.
2. An azeotropic dehydration method of acetic acid suitable for producing trimellitic anhydride, comprising the following steps:
step 1: the azeotropic distillation dilute acetic acid raw material liquid with the concentration of 80-85 percent enters an azeotropic distillation tower (T1) after being preheated to 80+/-5 ℃, isopropyl acetate is added into the tower to serve as an entrainer, the pressure in the tower bottom is controlled at 40-60 kpa, the temperature of the tower top is controlled at 52-60 ℃, and the temperature of the tower bottom is controlled at 100-110 ℃ through a reboiler so as to separate components with different boiling points;
step 2: acetic acid with the concentration of 96% extracted from the bottom of the azeotropic distillation tower (T1) enters an acetic acid product storage tank, gas-phase dilute acetic acid, water and entrainer at the top of the azeotropic distillation tower (T1) are condensed by a condenser I (E1) and enter an oil-water phase separation tank (D2) for phase separation, an oil phase flows back into the azeotropic distillation tower (T1) through an oil phase distribution pump (P2) and a distribution line V (X5), a water phase is output through a reflux distribution pump (P3) and then partially returns to the top of the azeotropic distillation tower (T1) through a valve III (V3), and the rest enters a solvent recovery tower (T2) through a valve IV (V4) for re-separation;
step 3: the gas phase at the top of the solvent recovery tower (T2) enters a liquid-liquid phase-splitting tank (D3) after being condensed by a condenser II (E2), PSC and IPA are separated in the liquid-liquid phase-splitting tank (D3) after liquid-liquid phase splitting and respectively enter a PSC intermediate storage tank (D4) and an IPA intermediate storage tank (D1), and the recovered material of the IPA intermediate storage tank (D1) returns to the oil phase partition of the oil-water phase-splitting tank (D2) through a reflux distribution pump (P1) and a distribution line I (X1).
3. The azeotropic dehydration process of acetic acid suitable for producing trimellitic anhydride as set forth in claim 2, wherein: in the step 2, the flow rate of the water phase returned from the oil-water phase separation tank (D2) to the top of the azeotropic distillation tower (T1) is equal to that of the oil phase by controlling a valve III (V3).
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| CN101704734A (en) * | 2009-11-20 | 2010-05-12 | 南京昂扬化工有限公司 | Method for recovering diluted acetic acid in production process of trimellitic anhydride |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
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| CN212246831U (en) * | 2020-06-10 | 2020-12-29 | 安庆亿成化工科技有限公司 | Acetic acid azeotropic dehydration device suitable for producing trimellitic anhydride |
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| US8382961B2 (en) * | 2010-06-07 | 2013-02-26 | Amt International, Inc. | System and method for reduction of water consumption in purified terephthalic acid production |
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| CN101704734A (en) * | 2009-11-20 | 2010-05-12 | 南京昂扬化工有限公司 | Method for recovering diluted acetic acid in production process of trimellitic anhydride |
| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
| CN104844444A (en) * | 2015-03-26 | 2015-08-19 | 南京师范大学 | Method for extracting acetic acid in salt-containing acetic acid aqueous solution by one-sided line heat integration azeotropic rectification method |
| CN212246831U (en) * | 2020-06-10 | 2020-12-29 | 安庆亿成化工科技有限公司 | Acetic acid azeotropic dehydration device suitable for producing trimellitic anhydride |
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