CN111643915B - Rectification device and rectification method for oxo-synthesis of acetic acid - Google Patents
Rectification device and rectification method for oxo-synthesis of acetic acid Download PDFInfo
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- CN111643915B CN111643915B CN201910853962.4A CN201910853962A CN111643915B CN 111643915 B CN111643915 B CN 111643915B CN 201910853962 A CN201910853962 A CN 201910853962A CN 111643915 B CN111643915 B CN 111643915B
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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
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/10—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide
- C07C51/12—Preparation of carboxylic acids or their salts, halides or anhydrides by reaction with carbon monoxide on an oxygen-containing group in organic compounds, e.g. alcohols
Abstract
The invention relates to a rectifying device for oxo-synthesis of acetic acid, which is internally provided with a partition plate (1) for bulkhead rectification of crude acetic acid in the oxo-synthesis of acetic acid, wherein the partition plate (1) is vertically arranged between a tower top rectifying section and a tower bottom stripping section, so that spaces at two sides of the partition plate (1) respectively form a first rectifying area (2) and a second rectifying area (3); the bottom end and the top end of the first rectifying area (2) and the second rectifying area (3) are communicated to form a common rectifying section (4) and a common stripping section (5); the first rectifying area (2) is provided with a crude acetic acid feeding hole (21) and a methanol injection assembly (22); the second rectifying area (3) is provided with a high-purity acetic acid discharge hole (31). Compared with the prior art, the purity of the acetic acid product reaches the excellent grade, and the energy consumption is reduced to 0.5-0.8t steam/t acetic acid compared with 1.8t steam/t acetic acid of three-tower rectification.
Description
Technical Field
The invention relates to a crude acetic acid rectification process, in particular to a rectification device and a rectification method for oxo-synthesis acetic acid.
Background
The traditional acetic acid device adopts three rectifying towers, namely, firstly removing light, then dehydrating (removing light for the second time), finally removing heavy, and collecting acetic acid from the tower top, the flow is long, the equipment is more, and the one-time investment of the acetic acid device is large due to high material requirement of producing acetic acid by carbonylation; on the other hand, two of the three rectifying towers need to use medium-pressure steam, about 1-1.8t of steam is consumed per ton of acetic acid, the energy consumption is high, and the acetic acid separation cost is high.
Therefore, there is a need to develop a high-efficiency energy-saving device and a specific rectification method suitable for oxo-synthesis of acetic acid, so as to realize industrial production.
CN107638709A discloses a separation device of acetic acid and water and its operation method. The device mainly comprises a dividing wall rectifying tower, a condenser, two reboilers and a delayer; the inside of the dividing wall rectifying tower is provided with a vertical partition plate, the lower end of the partition plate is closed, the upper end of the partition plate is communicated, the whole tower is divided into three areas, the upper part of the whole tower is a public rectifying area, and the lower part of the whole tower is a main tower stripping area and an auxiliary tower stripping area respectively. The process flow comprises the following steps: feeding the dilute acetic acid to be separated from the stripping area of the main tower, recovering pure acetic acid from the lower part of the dilute acetic acid for recycling, forming an azeotrope by water and an entrainer in a common rectification area, evaporating the azeotrope from the tower top, condensing the azeotrope into liquid, then layering the liquid in a delayer, pressurizing an oil phase, then refluxing the oil phase, pressurizing a water phase, then feeding the pressurized water phase into a stripping area of an auxiliary tower, rectifying and separating the mixture, recovering the entrainer in the common rectification area, and recovering wastewater from the stripping area of the auxiliary tower to discharge the system. The device and the process method are only suitable for acetic acid and water systems, adopt the simple partition wall tower with the lower end closed, are difficult to realize the specific requirements of the system in the aspects of design, discharging position and design of the partition wall tower and auxiliary tower in the case of the oxo-synthesis acetic acid system with complex components, are difficult to realize effective separation, and are incapable of treating hydrogen iodide in byproducts.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a rectification device and a rectification method for oxo-synthesis of acetic acid.
The purpose of the invention can be realized by the following technical scheme:
a rectifying device for oxo-synthesis of acetic acid is internally provided with a partition plate for bulkhead rectification of crude acetic acid in the oxo-synthesis of acetic acid, wherein the partition plate is vertically arranged between a tower top rectifying section and a tower bottom stripping section, so that spaces on two sides of the partition plate form a first rectifying area and a second rectifying area respectively;
the first rectifying area is communicated with the bottom end and the top end of the second rectifying area to form a public rectifying section and a public stripping section;
the first rectifying area is provided with a crude acetic acid feeding hole and a methanol injection assembly;
the second rectifying area is provided with a high-purity acetic acid discharge hole and a potassium hydroxide injection assembly;
the top of the public rectification section is provided with a condensation reflux assembly and a tower top discharge hole;
and a heater and a bottom heavy component liquid collecting tank are arranged at the bottom of the public stripping section.
Further, the methanol injection assembly comprises a methanol metering pump and a first automatic sampling port, the first automatic sampling port is externally connected with a first mass spectrum, the first mass spectrum is used for detecting the content of iodide ions in the crude acetic acid feeding port in real time, the first mass spectrum is connected with a computer terminal, and the computer terminal is used for sending a speed regulation instruction to a motor controller of the methanol metering pump.
Further, the potassium hydroxide injection assembly comprises a potassium hydroxide solution metering pump and a second automatic sampling port, a second mass spectrum is connected with the second automatic sampling port in an external mode, the second mass spectrum detects the content of iodide ions in the high-purity acetic acid discharge port in real time, and is connected with a computer terminal, and the computer terminal is used for sending a speed regulation instruction to a motor controller of the potassium hydroxide solution metering pump.
Further, the injection position of the methanol metering pump on the first rectification zone is lower than the crude acetic acid feed inlet;
the injection position of the potassium hydroxide solution metering pump on the second rectifying area is lower than the high-purity acetic acid discharge hole.
Furthermore, a liquid outlet is arranged on the bottom heavy component collecting tank.
Further, the total number of layers of the tower plates is 60-150.
Further, the first rectifying area or the second rectifying area accounts for 50-90% of the number of the plates.
Further, the methanol feed inlet is positioned on one of the 30-100 layers of tower plates.
The method for rectifying the crude acetic acid by utilizing the carbonyl synthesis of the rectifying device comprises the following steps:
s1: introducing crude acetic acid generated by synthesizing acetic acid by carbonyl into a crude acetic acid feeding hole, simultaneously opening a methanol injection assembly, and changing the injection flow of methanol in real time according to the concentration of hydrogen iodide obtained in real time to enable the methanol to react with the hydrogen iodide to generate methyl iodide; the flow of the injected potassium hydroxide solution is changed according to the content of iodine ions of the extracted acetic acid, so that potassium iodide is generated by the reaction of potassium hydroxide and the iodine ions and is accumulated in the heavy component collecting tank.
S2: collecting high-purity acetic acid through a high-purity acetic acid discharge port, and collecting water, methyl acetate, methyl iodide and non-condensable gas through a discharge port at the top of the tower;
s3: heavy components and potassium iodide are intermittently discharged through a liquid outlet on the liquid collecting and distributing box.
Further, the operating pressure in the rectifying tower is 5-200 KPa, the temperature at the top of the tower is controlled to be 80-130 ℃, the temperature of the tower kettle is 130-170 ℃, the feeding position of crude methanol is 30-100 layers, the feeding position of potassium hydroxide is 30-100 layers, and the discharging temperature of a high-purity acetic acid discharging port is 130-160 ℃.
In the specific rectification process, crude methanol firstly enters a first rectification zone from a crude acetic acid feeding hole, simultaneously methanol is introduced to react with hydrogen iodide to generate methyl iodide, and simultaneously potassium hydroxide is injected to enable iodide ions in acetic acid in a second rectification zone to reach a qualified level. Methyl acetate, methyl iodide, water and noncondensable gas are upwards enriched after carrying out layer-by-layer rectification in the first rectifying zone, acetic acid and heavy component are downwards enriched in the first rectifying zone and enter a public stripping section, and acetic acid and heavy component are separated layer by layer in the second rectifying zone, so that the heavy component is enriched to a tower kettle, and the acetic acid is upwards enriched and discharged from a high-purity acetic acid discharge port.
Compared with the prior art, the invention has the following advantages:
1) the process in the technical scheme adopts one tower to replace the original three towers, thereby greatly saving the equipment investment and the steam consumption which can be reduced by more than 60 percent. Is a new technology with high market competitiveness.
2) The first rectifying area and the second rectifying area are respectively provided with a methanol injection assembly and a potassium hydroxide injection assembly, and the maximum removal of iodide ions can be realized through the cooperation of the methanol injection assembly and the potassium hydroxide injection assembly with the partition tower.
3) The single tower adopted in the technical scheme replaces three towers, two zirconium material towers and four zirconium material heat exchangers are saved, the equipment investment is saved at 5000-10000 ten thousand yuan (taking 40 ten thousand ton scale as an example), the running steam and the circulating water are saved, and the function of separating three components in one tower is realized by utilizing the separation technology of the dividing wall tower.
4) The purity of the acetic acid product reaches the grade of superior products, and the energy consumption is reduced to 0.5-0.8t steam/t acetic acid compared with 1.8t steam/t acetic acid of three-tower rectification.
Drawings
FIG. 1 is a schematic view of a rectification apparatus for oxo acetic acid according to the present invention;
in the figure: 1. the device comprises a partition board, a first rectifying area, a second rectifying area, a first rectifying area, a second rectifying area, a third rectifying area, a fourth rectifying area, a fifth rectifying area, a high-purity acetic acid, a high purity acetic acid, a 32, a high purity acetic acid, a high purity, a high purity acetic acid, a high purity, a common rectifying area, 4, a common rectifying area.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
The utility model provides a rectifier unit for oxo acetic acid, inside is equipped with baffle 1 for the next door rectification of coarse acetic acid in the oxo acetic acid, baffle 1 locate perpendicularly between top of the tower rectifying section and the bottom stripping section for the space of 1 both sides of baffle forms first rectifying space 2 and second rectifying space 3 respectively. The total number of layers of the tower plates is 60-150. The first rectification zone 2 or the second rectification zone 3 accounts for 50-90% of the number of plates.
The first rectifying area 2 is communicated with the bottom end and the top end of the second rectifying area 3 to form a public rectifying section 4 and a public stripping section 5; the first rectifying area 2 is provided with a crude acetic acid feeding hole 21 and a methanol injection assembly 22; the second rectifying area 3 is provided with a high-purity acetic acid discharge port 31 and a potassium hydroxide injection assembly 32; a condensation reflux assembly and a tower top discharge hole 41 are arranged at the top of the public rectification section 4; the bottom of the common stripping section 5 is provided with a heater and a bottom heavies header tank 51. A liquid outlet is arranged on the bottom heavy component collecting tank 51.
The methanol injection assembly 22 comprises a methanol metering pump and a first automatic sampling port, the first automatic sampling port is externally connected with a first mass spectrum, the first mass spectrum detects the content of iodide ions in the crude acetic acid feed port 21 in real time, the first mass spectrum is connected with a computer terminal, and the computer terminal is used for sending a speed regulation instruction to a motor controller of the methanol metering pump. The injection position of the methanol metering pump on the first rectification zone 2 is lower than the crude acetic acid feed inlet 21
The potassium hydroxide injection assembly 32 comprises a potassium hydroxide solution metering pump and a second automatic sampling port, a second mass spectrum is externally connected to the second automatic sampling port, the second mass spectrum detects the content of iodine ions in the high-purity acetic acid discharge port 31 in real time, and is connected with a computer terminal, and the computer terminal is used for sending a speed regulation instruction to a motor controller of the potassium hydroxide solution metering pump. The injection position of a potassium hydroxide solution metering pump on the second rectifying area 3 is lower than the high-purity acetic acid discharge port 31.
The method for rectifying the crude acetic acid by utilizing the carbonyl synthesis of the rectifying device comprises the following steps:
s1: introducing crude acetic acid generated by synthesizing acetic acid by carbonyl into a crude acetic acid feeding hole 21, simultaneously opening a methanol injection assembly 22, and changing the injection flow of methanol in real time according to the concentration of hydrogen iodide obtained in real time to enable the methanol to react with the hydrogen iodide to generate methyl iodide; the flow rate of the injected potassium hydroxide solution is changed according to the content of iodine ions in the extracted acetic acid, so that potassium iodide is generated by the reaction of potassium hydroxide and iodine ions and accumulated in the heavy component header tank 51.
S2: collecting high-purity acetic acid through a high-purity acetic acid discharge port 31, and collecting water, methyl acetate, methyl iodide and non-condensable gas through a tower top discharge port 41;
s3: the heavy component and potassium iodide were intermittently discharged through a drain port in the liquid collection and collection tank 51.
The operating parameters are as follows: the operating pressure in the rectifying tower is 5-200 KPa, the temperature at the top of the tower is controlled to be 80-130 ℃, the temperature in the kettle of the tower is 130-170 ℃, the feeding position of crude methanol is 30-100 layers, the feeding position of potassium hydroxide is 30-100 layers, and the discharging temperature of a high-purity acetic acid discharging port 31 is 130-160 ℃.
In the specific rectification process, crude acetic acid generated by synthesizing acetic acid by carbonyl is introduced from a crude acetic acid feed inlet 21, a methanol injection component 22 is opened at the same time, crude methanol firstly enters a first rectification zone 2 from the crude acetic acid feed inlet 21, the injection flow of the methanol is changed in real time according to the concentration of hydrogen iodide obtained in real time, so that the methanol and the hydrogen iodide react to generate methyl iodide, and simultaneously potassium hydroxide is injected so that iodide ions are downward settled and enter a second rectification zone 3 to enable the iodide ions in the acetic acid to reach a qualified level; methyl acetate, methyl iodide, water and noncondensable gas are carried out layer by layer rectification in first rectifying zone and are enriched upwards, and acetic acid and heavy ends are enriched downwards in first rectifying zone and enter bottom heavy ends collection tank, get into public stripping section, and acetic acid and heavy ends are separated layer by layer in second rectifying zone 3 for the heavy ends are enriched to the tower cauldron, and acetic acid upwards enriches and follow the ejection of compact of high-purity acetic acid discharge gate. Collecting high-purity acetic acid through a high-purity acetic acid discharge port 31, and collecting water, acetic acid, methyl acetate, methyl iodide and non-condensable gas through a tower top discharge port 41; the heavy components and the enriched iodine ions are intermittently discharged through a liquid discharge port of the liquid collection and collection tank 51.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A rectifying device for oxo-synthesis of acetic acid is internally provided with a partition plate (1) for bulkhead rectification of crude acetic acid in the oxo-synthesis of acetic acid, and is characterized in that the partition plate (1) is vertically arranged between a tower top rectifying section and a tower bottom stripping section, so that spaces at two sides of the partition plate (1) form a first rectifying area (2) and a second rectifying area (3) respectively;
the bottom end and the top end of the first rectifying area (2) and the second rectifying area (3) are communicated to form a common rectifying section (4) and a common stripping section (5);
the first rectifying area (2) is provided with a crude acetic acid feeding hole (21) and a methanol injection assembly (22);
the second rectifying area (3) is provided with a high-purity acetic acid discharge hole (31) and a potassium hydroxide injection assembly (32), the injection position of a potassium hydroxide solution on the second rectifying area (3) is lower than the high-purity acetic acid discharge hole (31), and the injection position of methanol on the first rectifying area (2) is lower than the crude acetic acid feed hole (21);
the top of the public rectifying section (4) is provided with a condensation reflux assembly and a tower top discharge hole (41);
and a heater and a bottom heavy component collecting tank (51) are arranged at the bottom of the common stripping section (5).
2. The rectification device for oxo-acetic acid according to claim 1, wherein the methanol injection assembly (22) comprises a methanol metering pump and a first automatic sampling port, the first automatic sampling port is externally connected with a first mass spectrum, the first mass spectrum detects the content of iodide ions in the crude acetic acid feed port (21) in real time, the first mass spectrum is connected with a computer terminal, and the computer terminal is used for sending a speed regulation instruction to a motor controller of the methanol metering pump.
3. The rectification device for oxo-acetic acid according to claim 2, wherein the potassium hydroxide injection assembly (32) comprises a potassium hydroxide solution metering pump and a second automatic sampling port, the second automatic sampling port is externally connected with a second mass spectrum, the second mass spectrum detects the content of iodine ions in the high-purity acetic acid discharge port (31) in real time, the second mass spectrum is connected with a computer terminal, and the computer terminal is used for sending a speed regulation instruction to a motor controller of the potassium hydroxide solution metering pump.
4. A rectification unit for oxo acetic acid according to claim 3, wherein the injection position of the methanol metering pump in the first rectification zone (2) is lower than the crude acetic acid feed inlet (21);
the injection position of the potassium hydroxide solution metering pump on the second rectifying area (3) is lower than the high-purity acetic acid discharge hole (31).
5. A rectification apparatus for oxo acetic acid according to claim 1, wherein the bottom heavy fraction collection tank (51) is provided with a liquid drain.
6. A rectification apparatus for oxo acetic acid according to claim 1, wherein the total number of stages is 60 to 150.
7. A rectification apparatus for oxo acetic acid according to claim 6, wherein the first rectification zone (2) or the second rectification zone (3) occupies 50 to 90% of the number of plates.
8. A rectification apparatus for oxo acetic acid according to claim 6, wherein the methanol feed inlet (21) is located in one of 30 to 100 stages.
9. A method for rectifying crude acetic acid by oxo synthesis using the rectifying apparatus of claim 1, comprising the steps of:
s1: introducing crude acetic acid generated by synthesizing acetic acid by carbonyl into a crude acetic acid feeding hole (21) and simultaneously opening a methanol injection assembly (22), and changing the injection flow of methanol in real time according to the concentration of hydrogen iodide obtained in real time to enable the methanol to react with the hydrogen iodide to generate methyl iodide; the flow of injected potassium hydroxide solution is changed according to the content of iodine ions of the extracted acetic acid, so that potassium iodide is generated by the reaction of potassium hydroxide and the iodine ions and accumulated in a heavy component collecting tank (51);
s2: high-purity acetic acid is collected through a high-purity acetic acid discharge hole (31), and water, methyl acetate, methyl iodide and non-condensable gas are collected through a tower top discharge hole (41);
s3: the heavy components and potassium iodide are intermittently discharged through a liquid discharge port in the liquid collection and collection tank (51).
10. The method for rectifying the crude acetic acid for oxo synthesis according to claim 9, wherein the operating pressure in the rectifying tower is 5 to 200KPa, the temperature at the top of the rectifying tower is controlled to be 80 to 130 ℃, the temperature at the bottom of the rectifying tower is 130 to 170 ℃, the feeding position of the crude methanol is 30 to 100 layers, the feeding position of the potassium hydroxide is 30 to 100 layers, and the discharging temperature of the high-purity acetic acid discharging port (31) is 130 to 160 ℃.
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| CN201910853962.4A CN111643915B (en) | 2019-09-10 | 2019-09-10 | Rectification device and rectification method for oxo-synthesis of acetic acid |
| PCT/CN2020/111560 WO2021047393A1 (en) | 2019-09-10 | 2020-08-27 | Rectification device and rectification method for oxo synthesis of acetic acid |
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| CN201910853962.4A CN111643915B (en) | 2019-09-10 | 2019-09-10 | Rectification device and rectification method for oxo-synthesis of acetic acid |
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| CN113262516B (en) * | 2021-05-18 | 2022-06-24 | 河南中托力合化学有限公司 | Side-draw structure of baffle tower for separating C16-C19 normal paraffins |
| CN115318232B (en) * | 2022-07-12 | 2024-02-23 | 铜陵贝斯美科技有限公司 | Device and production process for co-producing amyl alcohol and methyl acetate |
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| CN1449369A (en) * | 2000-07-06 | 2003-10-15 | 米兰纽姆石化公司 | Process control for acetic acid manufacture |
| CN109534986A (en) * | 2017-09-21 | 2019-03-29 | 中国石油化工股份有限公司 | The method and apparatus of separating acetic acid from hexamethylene raw material |
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| DE19617210A1 (en) * | 1996-04-30 | 1997-11-06 | Basf Ag | Partition wall column for the continuous separation of multi-component mixtures by distillation |
| DE19914966A1 (en) * | 1999-04-01 | 2000-10-05 | Basf Ag | Process for the continuous distillative separation of a higher melting substance |
| DE10021624A1 (en) * | 2000-05-04 | 2001-11-08 | Basf Ag | Partition column |
| KR101146221B1 (en) * | 2009-02-12 | 2012-05-15 | 주식회사 엘지화학 | Dividing wall column |
| EP2502655B1 (en) * | 2011-03-25 | 2014-05-14 | Sulzer Chemtech AG | Reactive distillation process and plant for obtaining acetic acid and alcohol from the hydrolysis of methyl acetate |
| CN102690186A (en) * | 2012-06-12 | 2012-09-26 | 天津大学 | Methyl acetate hydrolysis partition reaction rectification column and operating method thereof |
| CN204637623U (en) * | 2015-04-13 | 2015-09-16 | 河南顺达化工科技有限公司 | Acetic acid rectifying and dewatering Tower System |
| CN107638709A (en) * | 2016-07-27 | 2018-01-30 | 中国石化仪征化纤有限责任公司 | The separator and its operating method of acetic acid and water |
| ES2792108T3 (en) * | 2017-02-07 | 2020-11-10 | Daicel Corp | Acetic acid production method |
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| US4039395A (en) * | 1975-08-11 | 1977-08-02 | Monsanto Company | Purification of acetic acid |
| CN1449369A (en) * | 2000-07-06 | 2003-10-15 | 米兰纽姆石化公司 | Process control for acetic acid manufacture |
| CN109534986A (en) * | 2017-09-21 | 2019-03-29 | 中国石油化工股份有限公司 | The method and apparatus of separating acetic acid from hexamethylene raw material |
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