CN210303605U - Can desorption corrosivity metal ion's acetic acid production system - Google Patents
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Abstract
An acetic acid production system capable of removing corrosive metal ions belongs to the technical field of acetic acid production processes. The acetic acid production system capable of removing corrosive metal ions comprises a reactor, a flash evaporator, a rectification system and a metal ion removal system. This system is through setting up metal ion desorption system, when guaranteeing that the normal qualified acetic acid product of production of device, effectively gets rid of the metal ion such as iron, chromium, manganese, nickel, calcium, magnesium in the reaction solution, and the removal rate of corrosive metal ion can reach more than 80%. The system can remove corrosive metal ions and simultaneously ensure that the metal rhodium ions of the catalyst and the metal lithium ions of the auxiliary agent do not generate large loss. After corrosive metal ions are removed by the metal ion removal system, the loss rate of metal rhodium ions (calculated by rhodium) of the catalyst can be reduced to 1-5%, and the loss rate of metal lithium ions (calculated by lithium) of the auxiliary agent is reduced to 1-5%.
Description
Technical Field
The utility model relates to an acetic acid production system capable of removing corrosive metal ions, which belongs to the technical field of acetic acid production process.
Background
The traditional methanol low-pressure carbonyl synthesis acetic acid system mainly comprises three systems of reaction, rectification and absorption. Because the reaction system uses HI and CH with high concentration3The I is used as a cocatalyst, and HI has strong corrosion to equipment in an aqueous environment. The materials such as zirconium material, hastelloy, stainless steel and the like adopted by the acetic acid production device contain metals such as iron, chromium, manganese, nickel and the like. When the system runs in a high-temperature acidic environment for a long time, equipment corrosion is enhanced, and metal ions such as iron, chromium, manganese, nickel and the like are gathered in the system. Meanwhile, if corrosion leakage occurs in the device and cooling water enters the system, calcium and magnesium ions can be accumulated in the system. When the concentration of metal ions is high to a certain degree (more than or equal to 3000ppm), the catalyst is easy to precipitate (namely Rh is obtained3+Conversion to RhI3) And the activity is lost, the system for synthesizing the acetic acid by the methanol low-pressure carbonyl is obviously deteriorated, the reaction speed is reduced, and the yield of the acetic acid is reduced.
A traditional methanol low-pressure oxo-synthesis acetic acid system is not provided with a metal ion removal device, and metal ions in the system can be removed only by precipitating a rhodium catalyst in reaction liquid, filtering liquid containing the metal ions, and dissolving the rhodium catalyst again for use. However, the lithium complex ligand which is beneficial to the dissolution of the rhodium catalyst is added in the existing methanol production system, so that the rhodium catalyst is difficult to precipitate, and corrosive metal ions in the reaction system are difficult to remove by adopting the traditional mode, thereby reducing the production efficiency of the traditional methanol low-pressure oxo-synthesis acetic acid system.
Disclosure of Invention
For solving the problem that exists among the prior art, the utility model provides a can desorption corrosivity metal ion's acetic acid production system, this system has optimized on traditional low pressure oxo acetic acid device, has introduced the device of corrosivity metal ion desorption, has guaranteed rhodium catalyst's long-term stability.
The utility model provides a technical scheme that technical problem adopted is: an acetic acid production system capable of removing corrosive metal ions comprises a reactor, a flash evaporator and a rectification system, wherein a liquid outlet of the reactor is connected with an inlet of the flash evaporator, a bottom outlet of the flash evaporator is connected with a bottom reflux port of the reactor through a main pipeline, and the acetic acid production system further comprises a metal ion removal system. The rectification system comprises a light component removal tower, a dehydration tower, a heavy component removal tower and a gas stripping tower, wherein a gas outlet at the upper part of the flash evaporator is connected with an inlet of the light component removal tower, a liquid phase outlet at the top of the light component removal tower is connected to the reactor through a first reflux pipeline, a gas phase outlet at the upper part of the right side of the light component removal tower is connected with a torch discharge system, and a bottom outlet of the light component removal tower is merged into a main pipeline through a tower bottom reflux pipeline and then is connected to a bottom reflux port of; an outlet at the lower part of the right side of the light component removal tower is connected with an inlet of a dehydration tower, a liquid phase extraction outlet at the top of the dehydration tower is connected to a first reflux pipeline through an extraction pipeline, a bottom outlet of the dehydration tower is connected with a left inlet of a heavy component removal tower, a top outlet of the heavy component removal tower is connected with the first reflux pipeline, a finished product outlet at the right side of the heavy component removal tower is connected with an acetic acid product pipeline, a bottom outlet of the heavy component removal tower is connected with a left inlet of a stripping tower, a top outlet of the stripping tower is connected to a left inlet of the heavy component removal tower through a third reflux pipeline, and a right outlet; the liquid phase extraction outlet at the top of the dehydration tower is also provided with a second return pipeline, and the liquid phase extraction outlet is connected to the inlet of the dehydration tower through the second return pipeline; the metal ion removal system comprises a cooler, a filter, a first adsorption tower and a second adsorption tower, wherein a bottom outlet of the flash evaporator is connected with a left inlet of the cooler through a lateral line pipeline, a right outlet of the cooler is connected with a top inlet of the filter, a bottom outlet of the filter is connected with a bottom inlet of the first adsorption tower through a first adsorption valve, and is connected with a bottom inlet of the second adsorption tower through a second adsorption valve, a top outlet of the first adsorption tower is connected with an adsorption tower reflux pipeline through a third adsorption valve, and a top outlet of the second adsorption tower is connected with an adsorption tower reflux pipeline through a fourth adsorption valve; the reflux pipeline of the adsorption tower is connected to the bottom reflux port of the reactor through a main pipeline.
The adsorption tower comprises a first adsorption tower, a second adsorption tower, a grid, a resin cavity, a second liquid distributor, a second cleaning port and an adsorption tower top outlet, wherein the first adsorption tower and the second adsorption tower are connected in parallel, the first adsorption tower and the second adsorption tower are collectively called as the adsorption tower, the adsorption tower structurally comprises an adsorption tower bottom inlet, a first cleaning port, a first liquid distributor, the grid, the resin cavity, the second liquid distributor, the second cleaning port and the adsorption tower top outlet, and a resin charging port and a resin discharging port are formed in the resin cavity.
The resin filled in the first adsorption tower and the second adsorption tower is macroporous strong acid type ion exchange resin, and the macroporous strong acid type ion exchange resin comprises ion exchange resin WET, ion exchange resin S, ion exchange resin or ion exchange resin LYS.
The filter is a metal sintered filter, a wire mesh filter or a ceramic sintered filter.
The corrosive metal ions include Fe2+、Cr2+、Mn2+、Ni2+、Ca2+And Mg2+ 。
The utility model has the advantages that: the acetic acid production system capable of removing corrosive metal ions comprises a reactor, a flash evaporator, a rectification system and a metal ion removal system. The rectification system comprises a light component removing tower, a dehydration tower, a heavy component removing tower and a stripping tower. The metal ion desorption system contains the cooler, the filter, first adsorption tower and second adsorption tower, the left side entry of side line pipe connection cooler is passed through to flash vessel bottom export, the top entry of the right side exit linkage filter of cooler, the bottom entry of first adsorption tower is connected through first adsorption valve to the bottom export of filter, the bottom entry of second adsorption tower is connected through second adsorption valve, the top export of first adsorption tower passes through third adsorption valve and connects the backflow pipeline, the top export of second adsorption tower passes through fourth adsorption valve and connects adsorption tower backflow pipeline. This acetic acid production system is through setting up metal ion desorption system, when guaranteeing that the normal qualified acetic acid product of production of device, gets rid of metal ions such as iron, chromium, manganese, nickel, calcium, magnesium in the reaction liquid. The system can remove corrosive metal ions in the reaction liquid and simultaneously ensure that the metal rhodium ions of the catalyst and the metal lithium ions of the auxiliary agent do not generate large loss. After corrosive metal ions are removed by the metal ion removal system, the loss rate of metal rhodium ions (calculated by rhodium) of the catalyst can be reduced to 1-5%, and the loss rate of metal lithium ions (calculated by lithium) of the auxiliary agent is reduced to 1-5%.
Drawings
FIG. 1: is a structural diagram of an acetic acid production system capable of removing corrosive metal ions.
FIG. 2: is a partially enlarged view of the first adsorption tower in fig. 1.
In the figure: 1. a reactor; 2. a flash evaporator; 2a, a main pipeline; 2b, a lateral line pipeline; 3. a light component removal tower; 3a, a first return pipeline; 3b, a tower bottom reflux pipeline, 4, a dehydration tower; 4a, a production pipeline; 4b, a second return pipeline; 5. a de-weighting tower; 6. a stripper column; 6a, a third return pipeline; 7. a cooler; 8. a filter; 9. a first adsorption tower; 9a, a first adsorption valve; 9b, a third adsorption valve; 9c1An inlet at the bottom of the adsorption tower; 9c2An outlet at the top of the adsorption tower; 9d1A first cleaning opening; 9d2A second cleaning port; 9e, a first liquid distributor; 9f, grid; 9g, resin cavity; 9g of1A resin charging port; 9g of2A resin discharge port; 9h, a second liquid distributor; 10. a second adsorption column; 10a, a second adsorption valve; 10b a fourth adsorption valve; 10c, a reflux pipeline of the adsorption tower.
Detailed Description
The technical details of the present invention will be further explained with reference to the accompanying drawings.
Fig. 1 shows a structural diagram of an acetic acid production system capable of removing corrosive metal ions, wherein the acetic acid production system capable of removing corrosive metal ions comprises a reactor 1, a flash evaporator 2 and a rectification system, a liquid outlet of the reactor 1 is connected with an inlet of the flash evaporator 2, a bottom outlet of the flash evaporator 2 is connected with a bottom reflux port of the reactor 1 through a main pipe 2a, and the acetic acid production system further comprises a metal ion removal system. The rectification system comprises a light component removal tower 3, a dehydration tower 4, a heavy component removal tower 5 and a stripping tower 6, a gas outlet at the upper part of the flash evaporator 2 is connected with an inlet of the light component removal tower 3, a liquid phase outlet at the top of the light component removal tower 3 is connected to the reactor 1 through a first reflux pipeline 3a, a gas phase outlet at the upper part of the right side of the light component removal tower 3 is connected with a torch discharge system, and a bottom outlet of the light component removal tower 3 is connected to a bottom reflux port of the reactor 1 after being merged into a main pipeline 2a through a tower bottom reflux pipeline 3 b. The entry of the exit linkage dehydration tower 4 of 3 right side lower parts in the light tower that takes off, the liquid phase of 4 tops in dehydration tower is adopted the export and is connected to first return line pipeline 3a through extraction pipeline 4a, the left side entry of the bottom exit linkage heavy tower 5 of dehydration tower 4, the top exit linkage first return line pipeline 3a of the heavy tower 5 that takes off, the finished product exit linkage acetic acid product pipeline on the heavy tower 5 right side that takes off, the left side entry of the bottom exit linkage stripper 6 of the heavy tower 5 that takes off, the top export of stripper 6 is connected to the left side entry of the heavy tower 5 that takes off through third return line 6a, the right side exit linkage waste acid pipeline of stripper 6. The liquid phase extraction outlet at the top of the dehydrating tower 4 is also provided with a second return pipeline 4b, and the liquid phase extraction outlet is connected to the inlet of the dehydrating tower 4 through the second return pipeline 4 b. The metal ion removal system comprises a cooler 7, a filter 8, a first adsorption tower 9 and a second adsorption tower 10, wherein a bottom outlet of the flash evaporator 2 is connected with a left inlet of the cooler 7 through a lateral line pipeline 2b, a right outlet of the cooler 7 is connected with a top inlet of the filter 8, a bottom outlet of the filter 8 is connected with a bottom inlet of the first adsorption tower 9 through a first adsorption valve 9a, the bottom outlet of the second adsorption tower 10 is connected with a bottom inlet of the second adsorption tower 10 through a second adsorption valve 10a, a top outlet of the first adsorption tower 9 is connected with an adsorption tower reflux pipeline 10c through a third adsorption valve 9b, and a top outlet of the second adsorption tower 10 is connected with an adsorption tower reflux pipeline 10c through a fourth adsorption valve 10 b. The adsorption tower reflux line 10c is connected to the bottom reflux port of the reactor 1 via the main line 2 a.
The first adsorption tower 9 and the second adsorption tower 10 are connected in parallel, the first adsorption tower 9 and the second adsorption tower 10 are collectively called an absorption tower, and the absorption tower has a structure including an inlet 9c at the bottom of the absorption tower1The first cleaning port 9d1A first liquid distributor 9e, a grid 9f, a resin cavity 9g, a second liquid distributor 9h, and a second cleaning port 9d2And an outlet 9c at the top of the adsorption column2 A resin inlet 9g is provided in the resin chamber 9g1And a resin discharge port 9g2。
The resin packed in the first adsorption tower 9 and the second adsorption tower 10 is macroporous strong acid type ion exchange resin, and the macroporous strong acid type ion exchange resin comprises ion exchange resin 15WET, ion exchange resin S30, ion exchange resin 608 or ion exchange resin LYS.
The filter 8 is a metal sintered filter, a wire mesh filter or a ceramic sintered filter.
The corrosive metal ions include Fe2+、Cr2+、Mn2+、Ni2+、Ca2+And Mg2+ 。
The specific production flow of the acetic acid production system capable of removing the corrosive metal ions comprises the following steps: methanol and CO enter a reactor 1, are mixed and react under the action of a rhodium catalyst to generate acetic acid, reaction liquid containing the acetic acid enters a flash evaporator 2 through a liquid outlet of the reactor 1 to be subjected to reduced pressure flash evaporation, gas-phase components obtained by flash evaporation comprise products of acetic acid, water, methyl iodide, methyl acetate and the like and enter a rectification system, the gas phase component firstly enters a light component removal tower 3, the removed light components such as methyl iodide, methyl acetate, methanol and the like are condensed and then returned to the reactor 1 from the outlet of the top of the light component removal tower 3 through a first reflux pipeline 3a, the light component after being removed enters a dehydration tower 4 to remove moisture, then enters a de-heavy tower 5 and a stripping tower 6 to remove heavy components such as propionic acid and the like to finally obtain a qualified acetic acid product, the finished acetic acid product enters an acetic acid product pipeline system, and gas discharged from a gas phase outlet at the upper part of the right side of the light component removal tower 3 enters a torch discharge system. From the bottom outlet of the flash evaporator 2, a part of the catalyst and other non-gasified components are returned to the reactor 1 through a main pipe 2a, and the rest enters a metal ion removal system through a side pipe 2b for metal ion removal. The liquid phase component extracted from the side line of the outlet at the bottom of the flash evaporator 2 is the conventional reaction mother liquor, the partial reaction liquid is cooled by a cooler 7 and then enters a filter 8, impurities such as solid particles and tar in the liquid are removed by the filter 8, the filtered liquid enters an adsorption tower, metal ions such as iron, chromium, manganese, nickel, calcium, magnesium and the like dissolved in the liquid are removed by resin adsorption, the liquid from which the metal ions are removed returns to the reactor 1 through a reflux pipeline 10c of the adsorption tower, and the circulation is carried out, so that the content of the metal ions such as iron, chromium, manganese, nickel, calcium, magnesium and the like in the whole acetic acid production system is removed to a qualified index.
The utility model discloses a metal ion desorption system adopts the parallelly connected structural style of first adsorption tower 9 and second adsorption tower 10, two adsorption towers use in turn, when first adsorption tower 9 need change resin or saturation need be regenerated, close first adsorption valve 9a and third adsorption valve 9b, stop using first adsorption tower 9, open second adsorption valve 10a and fourth adsorption valve 10b, intercommunication second adsorption tower 10 carries out metal ion's absorption, this kind of structural style has avoided the shut-down phenomenon because of changing the adsorption tower resin and leading to, the production efficiency of this acetic acid production system has been improved. The first adsorption tower 9 and the second adsorption tower 10 have the same structure, and the resin replacement and the resin regeneration are performed in the same manner. The process of resin replacement or regeneration will be described by taking the first adsorption tower 9 as an example. The process of replacing the resin in the first adsorption tower 9 is as follows: opening the resin discharge port 9g2After discharging the old resin, the resin discharge port 9g is closed2Opening the first cleaning port 9d1And a second cleaning port 9d2Opening the resin inlet 9g1Filling the new resin. The regeneration process of the resin in the first adsorption tower 9 comprises the following steps: the first cleaning port 9d is opened1And a second cleaning port 9d2The first adsorption tower 9 is washed with water, and the resin in the resin chamber 9g is regenerated with a regeneration solution after being washed clean.
The adsorption temperature of the resin in the adsorption tower can be adjusted between 10 ℃ and 100 ℃, the adsorption pressure can be from normal pressure to 40MPa, and the removal rate of corrosive metal ions can reach more than 80%. After corrosive metal ions are removed, the loss rate of metal rhodium ions (calculated as rhodium) of the catalyst is reduced to 1-5%, and the loss rate of metal lithium ions (calculated as lithium) of the auxiliary agent is reduced to 1-5%.
Specific metal ion removal examples are given below in connection with the actual production of such a corrosive metal ion removable acetic acid production system:
example 1: the adsorption tower is filled with ion exchange resin 15WET
Temperature: 30 ℃, flow rate: 0.5m3H, amount of treatment reaction liquid: 1m3And the loading of resin in the adsorption tower: 2m3。
Example 1 Metal ion removal data sheet
Example 2 adsorption column packing with ion exchange resin S30
Temperature: 30 ℃, flow rate: 0.5m3H, amount of treatment reaction liquid: 1m3And the loading of resin in the adsorption tower: 2m3。
Example 2 Metal ion removal data sheet
Example 3: the adsorption column is filled with ion exchange resin 608
Temperature: 50 ℃, flow rate: 1m3H, amount of treatment reaction liquid: 2m3And the loading of resin in the adsorption tower: 5m3。
Example 3 Metal ion removal data Table
Example 4: the adsorption tower is filled with ion exchange resin LYS
Temperature: 40 ℃, flow rate: 1m3H, amount of treatment reaction liquid: 2m3And the loading of resin in the adsorption tower: 5m3。
Example 4 Metal ion removal data Table
Claims (5)
1. An acetic acid production system capable of removing corrosive metal ions comprises a reactor (1), a flash evaporator (2) and a rectification system, wherein a liquid outlet of the reactor (1) is connected with an inlet of the flash evaporator (2), and a bottom outlet of the flash evaporator (2) is connected with a bottom reflux inlet of the reactor (1) through a main pipeline (2 a), and is characterized by further comprising a metal ion removal system;
the rectification system comprises a light component removal tower (3), a dehydration tower (4), a heavy component removal tower (5) and a stripping tower (6), a gas outlet at the upper part of the flash evaporator (2) is connected with an inlet of the light component removal tower (3), a liquid phase outlet at the top of the light component removal tower (3) is connected to the reactor (1) through a first reflux pipeline (3 a), a gas phase outlet at the upper part of the right side of the light component removal tower (3) is connected with a torch discharge system, and a bottom outlet of the light component removal tower (3) is merged into a main pipeline (2 a) through a tower bottom reflux pipeline (3 b) and then is connected to a bottom reflux port of the reactor (1); an outlet at the lower part of the right side of the light component removal tower (3) is connected with an inlet of a dehydration tower (4), a liquid phase extraction outlet at the top of the dehydration tower (4) is connected to a first reflux pipeline (3 a) through an extraction pipeline (4 a), a bottom outlet of the dehydration tower (4) is connected with a left inlet of a heavy component removal tower (5), a top outlet of the heavy component removal tower (5) is connected with the first reflux pipeline (3 a), a finished product outlet at the right side of the heavy component removal tower (5) is connected with an acetic acid product pipeline, a bottom outlet of the heavy component removal tower (5) is connected with a left inlet of an air stripping tower (6), a top outlet of the air stripping tower (6) is connected to a left inlet of the heavy component removal tower (5) through a third reflux pipeline (6 a), and a right outlet of the air stripping tower; the liquid phase extraction outlet at the top of the dehydration tower (4) is also provided with a second reflux pipeline (4 b), and the liquid phase extraction outlet is connected to the inlet of the dehydration tower (4) through the second reflux pipeline (4 b);
the metal ion removal system comprises a cooler (7), a filter (8), a first adsorption tower (9) and a second adsorption tower (10), wherein a bottom outlet of the flash evaporator (2) is connected with a left inlet of the cooler (7) through a lateral line pipeline (2 b), a right outlet of the cooler (7) is connected with a top inlet of the filter (8), a bottom outlet of the filter (8) is connected with a bottom inlet of the first adsorption tower (9) through a first adsorption valve (9 a), is connected with a bottom inlet of the second adsorption tower (10) through a second adsorption valve (10 a), a top outlet of the first adsorption tower (9) is connected with an adsorption tower reflux pipeline (10 c) through a third adsorption valve (9 b), and a top outlet of the second adsorption tower (10) is connected with an adsorption tower reflux pipeline (10 c) through a fourth adsorption valve (10 b); the reflux pipeline (10 c) of the adsorption tower is connected to the bottom reflux port of the reactor (1) through a main pipeline (2 a).
2. The acetic acid production system capable of removing corrosive metal ions according to claim 1, wherein the first adsorption tower (9) and the second adsorption tower (10) are connected in parallel, the first adsorption tower (9) and the second adsorption tower (10) are collectively called an absorption tower, and the structure of the absorption tower comprises an inlet (9 c) at the bottom of the absorption tower1) A first cleaning opening (9 d)1) A first liquid distributor (9 e), a grid (9 f), a resin cavity (9 g), a second liquid distributor (9 h), and a second cleaning opening (9 d)2) And an outlet (9 c) at the top of the adsorption column2) The resin cavity (9 g) is provided with a resin inlet (9 g)1) And a resin discharge port (9 g)2）。
3. The acetic acid production system capable of removing corrosive metal ions according to claim 1, wherein the first adsorption tower (9) and the second adsorption tower (10) are filled with resins of macroporous strong acid type, and the macroporous strong acid type ion exchange resins comprise ion exchange resin 15WET, ion exchange resin S30, ion exchange resin 608 or ion exchange resin LYS.
4. The acetic acid production system capable of removing corrosive metal ions according to claim 1, wherein the filter (8) is a metal sintered filter, a wire mesh filter or a ceramic sintered filter.
5. The acetic acid production system with corrosive metal ions removed according to claim 1, wherein the corrosive metal ions comprise Fe2+、Cr2+、Mn2+、Ni2+、Ca2+And Mg2+。
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| CN114213238A (en) * | 2021-12-09 | 2022-03-22 | 河南神马尼龙化工有限责任公司 | Preparation method for reducing iron ion content in refined adipic acid product |
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| CN114213238A (en) * | 2021-12-09 | 2022-03-22 | 河南神马尼龙化工有限责任公司 | Preparation method for reducing iron ion content in refined adipic acid product |
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Effective date of registration: 20220922 Address after: No. 282, Commercial Area 2B, 4th Floor, Building 1, Yinhai Polaris, No. 66, Jiayuan Road, Longxi Street, Yubei District, Chongqing 401120 Patentee after: Chongqing Daowei Low Carbon Technology Co.,Ltd. Address before: Room 185, floor 1, building 2, No. 1, Anhua street, Konggang street, Shunyi District, Beijing 100101 Patentee before: YUGE (BEIJING) TECHNOLOGY Co.,Ltd. |
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