CN111111312A - Device for recovering suspended particles in PTA oxidation mother liquor and using method thereof - Google Patents
Device for recovering suspended particles in PTA oxidation mother liquor and using method thereof Download PDFInfo
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- CN111111312A CN111111312A CN202010069616.XA CN202010069616A CN111111312A CN 111111312 A CN111111312 A CN 111111312A CN 202010069616 A CN202010069616 A CN 202010069616A CN 111111312 A CN111111312 A CN 111111312A
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- Prior art keywords
- filter
- mother liquor
- clear liquid
- collecting tank
- valve
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- 239000012452 mother liquor Substances 0.000 title claims abstract description 106
- 239000002245 particle Substances 0.000 title claims abstract description 43
- 230000003647 oxidation Effects 0.000 title claims abstract description 23
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 72
- 238000001914 filtration Methods 0.000 claims abstract description 39
- 239000007787 solid Substances 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 21
- 239000012528 membrane Substances 0.000 claims abstract description 18
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000009295 crossflow filtration Methods 0.000 claims abstract description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 33
- 230000001105 regulatory effect Effects 0.000 claims description 20
- 230000002378 acidificating effect Effects 0.000 claims description 8
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 8
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 230000008676 import Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 10
- 239000012065 filter cake Substances 0.000 abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004537 pulping Methods 0.000 abstract description 3
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 30
- 230000004907 flux Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000005711 Benzoic acid Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- FXLOVSHXALFLKQ-UHFFFAOYSA-N p-tolualdehyde Chemical compound CC1=CC=C(C=O)C=C1 FXLOVSHXALFLKQ-UHFFFAOYSA-N 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/02—Combinations of filters of different kinds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D35/00—Filtering devices having features not specifically covered by groups B01D24/00 - B01D33/00, or for applications not specifically covered by groups B01D24/00 - B01D33/00; Auxiliary devices for filtration; Filter housing constructions
- B01D35/16—Cleaning-out devices, e.g. for removing the cake from the filter casing or for evacuating the last remnants of liquid
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a device for recovering suspended particles in PTA oxidation mother liquor and a using method thereof, wherein the device comprises a filter press, a filter, a clear liquid collecting tank and a mother liquor collecting tank; the filter press and the mother liquor collecting tank are connected through a mother liquor main pipe, the filter press is connected with one end of a filter through a branch pipe, the membrane surface of a filter element of the filter is connected with an acid inlet pipeline, the other end of the filter is connected with the mother liquor collecting tank through a pipeline, the filter element is connected with a clear liquid collecting tank through a clear liquid outlet pipe, the clear liquid outlet pipe is provided with a clear liquid outlet valve, and the using method of the device comprises a mother liquor extracting stage, a filtering stage adopting a cross flow filtering mode and an acid washing. The invention adopts a cross-flow filtration mode, the filtration precision is 10-40nm, solid suspended particles in the PTA mother liquor are recovered to the maximum extent, the filter has higher corrosion resistance, the process of pulping filter cakes due to the formation of the filter cakes by the solid particles is omitted, the process is simplified, the production cost and the operation cost of the device are reduced, and the use effect is stable.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a device for recovering suspended particles in PTA oxidation mother liquor and a using method thereof.
Background
In the PTA production process, a certain amount of oxidation mother liquor is formed, and the mother liquor contains organic matters such as terephthalic acid, benzoic acid, p-methyl benzaldehyde and the like and a certain amount of catalyst. The recovery of solid organic matters can save material loss and production cost.
The early PTA oxidation mother liquor filtration adopts a bag filter or a metal sintering filter, the operation mode adopts a dead-end mode, mainly cake formation is carried out, then high-pressure gas is used for backflushing and blanking, and the collected slurry is pulped and sent back to the system. The method has the advantages of multiple process links and high operating cost, and simultaneously, the slurry form is returned to the PTA production system, which easily causes the problem of short-time system concentration fluctuation and influences the product quality.
Meanwhile, the main component of the PTA oxidation mother liquor is high-temperature acetic acid with the concentration of more than 90%, the PTA oxidation mother liquor can not be used for a long time in a bag type and a metal material, and the conditions of filter element damage, cracking and the like occur on site in actual operation of a factory. And the filtration precision of the two filtration systems can only be controlled to be 0.5 micron, and part of particulate matters can not be intercepted, thereby causing loss.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects of low filtration precision and large filter loss of solid suspended particles in PTA oxidation mother liquor in the prior art, the invention discloses a device for recovering suspended particles in PTA oxidation mother liquor and a using method thereof, wherein the existing dead-end filtration is replaced by a cross flow mode, the filtration precision is 10-40nm, and the solid suspended particles in the PTA mother liquor are recovered to the maximum extent.
The technical scheme is as follows: the invention discloses a device for recovering suspended particles in PTA oxidation mother liquor, which comprises a filter press, a filter, a clear liquid collecting tank and a mother liquor collecting tank, wherein the filter press is arranged on the filter press; pressure filter and mother liquor collecting tank pass through the mother liquor house steward and link to each other, be equipped with mother liquor import governing valve on the mother liquor house steward, the pressure filter passes through the tributary pipe and links to each other with filter one end, the tributary pipe is equipped with filter inlet valve, filter core face links to each other with entering sour pipeline, it is equipped with into sour valve on the sour pipeline to advance, the filter other end passes through the pipeline and links to each other with the mother liquor collecting tank, be equipped with filter export governing valve on the pipeline, it links to each other with the clear liquid collecting tank through.
Preferably, the acid liquid is introduced into the acid inlet pipeline and flows into the membrane surface of the filter element of the filter, solid particles left by the membrane surface of the filter element during filtration are dissolved, and the flow rate of the membrane surface in the filter is 0.5-1.2 m/s.
Preferably, a clear liquid diversion groove is formed in the side face of the filter and connected with a clear liquid outlet pipe.
Preferably, the filter is a silicon carbide filter.
Preferably, the filter element in the filter is a 100% recrystallized silicon carbide sintered filter element.
Preferably, the filter has a filtration precision of 10-40 nm.
Preferably, the acidic liquid introduced into the acid inlet pipeline is an acetic acid solution, the concentration of the acetic acid is over 90%, and the temperature is over 80 ℃.
The use method of the device for recovering suspended particles in PTA oxidation mother liquor comprises the following steps:
step A, mother liquor extraction stage: opening a main mother liquor loop; the filter press extracts PTA mother liquor in the mother liquor collecting tank to enter a mother liquor main pipe, a mother liquor inlet adjusting valve is opened, and the PTA mother liquor enters the mother liquor collecting tank;
step B, a filtering stage: closing the main mother liquor loop and opening the filtering branch; opening an inlet valve of a filter, closing a mother liquor inlet adjusting valve, introducing PTA mother liquor into the filter, enabling the filter to pass through a cross flow filtration mode, enabling the PTA mother liquor to flow into a mother liquor collecting tank from a pipeline along the direction of a filter element of the filter, and enabling clear liquor to flow into a clear liquor outlet pipe from a clear liquor diversion trench; when the pressure value in the pipeline exceeds 0.25Mpa, opening a clear liquid outlet valve, allowing clear liquid to enter a clear liquid collecting tank through the clear liquid outlet valve, and leaving solid suspended particles in the filter;
step C, acid washing stage: when the pressure value in the pipeline exceeds 0.4Mpa, opening the main mother liquor loop and the pickling loop, and closing the filtering branch; opening a mother liquor inlet regulating valve, closing a filter inlet valve, a clear liquid outlet valve and a filter outlet regulating valve, then opening an acid inlet valve, enabling the acidic liquid to enter a filter and wash and dissolve solid particles left by the filter element during filtering, and fully opening the filter outlet regulating valve after washing, so that the acidic liquid with the dissolved solid particles flows into a mother liquor collecting tank, and returning to the step A.
Preferably, the step B includes:
step B1, closing the mother liquid main loop, opening the filtering branch: opening a filter inlet valve, fully opening a filter outlet regulating valve, and closing a mother liquor inlet regulating valve after a period of time;
step B2, entering a filtering stage: setting a filter outlet regulating valve as an automatic mode, and starting to filter and time-count PTA mother liquor;
step B3, clear liquid receiving stage: when the pressure value in the pipeline exceeds 0.25MPa, the clear liquid outlet valve is opened, clear liquid enters the clear liquid collecting tank through the clear liquid outlet valve, and solid suspended particles are left in the filter.
Has the advantages that:
1. the filter adopts a cross-flow filtration mode to replace the existing dead-end filtration mode, the filtration precision is 10-40nm, solid suspended particles in the PTA mother liquor are recovered to the maximum extent, the process of pulping filter cakes due to the formation of the filter cakes by the solid particles is omitted, the process is simplified, the production cost and the operation cost of the device are reduced, and the use effect is stable;
2. the silicon carbide filter is adopted, so that the corrosion resistance is extremely high, and the service life is long;
3. the invention also comprises an acid washing process, acetic acid is adopted for back flushing, the acetic acid is utilized for dissolving suspended particles, the back flushing process is soft, the back-flushed concentrated solution is directly returned to the PTA system, the suspended particles are recycled, the production cost is reduced, and the membrane flux of the filter is effectively recovered;
4. the invention realizes the filtering function by utilizing the power provided by the filter press without additionally arranging a pump.
Drawings
FIG. 1 is a schematic view of the general structure of the present invention;
wherein 1 is a filter press, 2 is a mother liquor inlet regulating valve, 3 is a filter inlet valve, 4 is an acid inlet valve, 5 is a filter, 51 is a clear liquid diversion trench, 6 is a clear liquid outlet valve, 7 is a clear liquid collecting tank, 8 is a filter outlet regulating valve, and 9 is a mother liquor collecting tank;
FIG. 2 is a schematic view of a filter cross-flow filtration mode of the present invention;
FIG. 3 is a flow chart of the present invention.
Detailed Description
The scheme is further explained by combining the attached drawings.
As shown in the attached figure 1, the device for recovering suspended particles in PTA oxidation mother liquor comprises a filter press 1, a filter 5, a clear liquid collecting tank 7 and a mother liquor collecting tank 9; pressure filter 1 and mother liquor collecting tank 9 link to each other through the mother liquor house steward, be equipped with mother liquor inlet governing valve 2 on the mother liquor house steward, pressure filter 1 links to each other through tributary pipe and 5 one ends of filter, tributary pipe is equipped with filter inlet valve 3, 5 filter core membrane faces of filter link to each other with advancing sour pipeline, it is equipped with into sour valve 4 on the sour pipeline to advance, 5 other ends of filter pass through pipeline and mother liquor collecting tank 9 and link to each other, be equipped with filter export governing valve 8 on the pipeline, 5 sides of filter link to each other with clear liquid collecting tank 7 through the clear liquid outlet pipe, the. The side of the filter 5 is provided with a clear liquid diversion groove 51, and the clear liquid diversion groove 51 is connected with a clear liquid outlet pipe. According to the scheme, the medium-pressure filter provides power for the whole device to realize the filtering function, the device does not need to be additionally provided with a pump, the process flow is reduced, and the production cost is reduced.
As shown in the attached figure 2, the filter 5 is a silicon carbide filter, the filter element of the filter 5 is a 100% recrystallized silicon carbide sintered filter element, a cross flow filtration mode is adopted, the PTA mother liquor flows into the mother liquor collecting tank 9 from a pipeline along the direction of the filter element of the filter 5, and the clear liquor flows out from the side surface of the filter element of the filter 5, flows into the clear liquor outlet pipe through the clear liquor diversion groove and enters the clear liquor collecting tank 7; the adoption of the cross flow filtration mode can not form filter cakes on the filter element membrane surface of the filter 5, and the membrane flux is reduced.
Acid liquid is introduced into the acid inlet pipeline and flows into the filter element membrane surface of the filter 5, solid particles left during filtering of the filter element membrane surface are dissolved, wherein the solid particles also contain production products which can be dissolved in the acid liquid, and the production products need to be recycled. The flow velocity of the membrane surface in the filter 5 is 0.5-1.2m/s, and the filtering precision of the filter 5 is 10-40 nm; the silicon carbide filter has extremely high corrosion resistance and long service life.
The acid liquid is introduced into the acid inlet pipeline and is an acetic acid solution, and the concentration of the acetic acid is over 90 percent. The temperature exceeds 80 ℃. Acetic acid is adopted for backflushing, suspended particles are dissolved by the acetic acid, the backflushing process is soft, the backflushed concentrated solution is directly returned to the PTA system, and the membrane flux of the filter 5 is effectively recovered.
As shown in the attached figure 3, the use method of the device for recovering suspended particles in PTA oxidation mother liquor comprises the following steps:
step A, mother liquor extraction stage: opening a main mother liquor loop; the filter press 1 extracts PTA mother liquor in the mother liquor collection tank 9 and enters a mother liquor main pipe, a mother liquor inlet adjusting valve 2 is opened, and the PTA mother liquor enters the mother liquor collection tank 9;
step B, a filtering stage: firstly, closing a mother liquor main loop and opening a filtering branch; opening the filter inlet valve 3, fully opening the filter outlet regulating valve 8, and closing the mother liquor inlet regulating valve 2 after a period of time; secondly, entering a filtering stage; setting a filter outlet regulating valve 8 to be in an automatic mode, starting to filter PTA mother liquor, leading the PTA mother liquor to flow into a mother liquor collecting tank 9 from a pipeline along the direction of a filter element of the filter 5 in a cross flow filtering mode by the filter 5, and leading clear liquid to flow into a clear liquid outlet pipe from a clear liquid diversion trench; finally, entering a clear liquid receiving stage; when the pressure value in the pipeline exceeds 0.25MPa, the clear liquid outlet valve 6 is opened, clear liquid enters the clear liquid collecting tank 7 through the clear liquid outlet valve 6, and solid suspended particles are left in the filter 5.
Step C, acid washing stage: when the pressure value in the pipeline exceeds 0.4Mpa, opening the main mother liquor loop and the pickling loop, and closing the filtering branch; opening the mother liquor inlet regulating valve 2, closing the filter inlet valve 3, the clear liquid outlet valve 6 and the filter outlet regulating valve 8, then opening the acid inlet valve 4, enabling the acidic liquid to enter the filter 5 and wash and dissolve solid particles left by the filter element membrane surface during filtration, and fully opening the filter outlet regulating valve 8 after washing, so that the acidic liquid with the dissolved solid particles flows into the mother liquor collecting tank 9, and returning to the step A.
The scheme adopts a cross-flow mode to replace the existing dead-end filtration mode, the filtration precision is 10-40nm, solid suspended particles in the PTA mother liquor are recovered to the maximum extent, the process of pulping filter cakes due to the formation of the filter cakes by the solid particles is omitted, the process is simplified, the production cost and the operation cost of the device are reduced, and the use effect is stable;
the above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (9)
1. The utility model provides a retrieve device of suspended particles in PTA oxidation mother liquor which characterized in that: comprises a filter press (1), a filter (5), a clear liquid collecting tank (7) and a mother liquid collecting tank (9); pressure filter (1) and mother liquor collecting tank (9) link to each other through the mother liquor house steward, be equipped with mother liquor import governing valve (2) on the mother liquor house steward, pressure filter (1) link to each other through tributary pipe and filter (5) one end, the tributary pipe is equipped with filter inlet valve (3), filter (5) filter core membrane face links to each other with entering sour pipeline, it is equipped with into sour valve (4) on the pipeline to advance, filter (5) other end passes through the pipeline and links to each other with mother liquor collecting tank (9), be equipped with filter export governing valve (8) on the pipeline, filter (5) side is passed through the clear liquid outlet pipe and is linked to each other with clear liquid collecting tank (7.
2. The apparatus of claim 1 for recovering suspended particles in PTA oxidation mother liquor, which is characterized in that: acidic liquid is introduced into the acid inlet pipeline and flows into the filter element membrane surface of the filter (5) to dissolve solid particles left during filtering of the filter element membrane surface, and the membrane surface flow velocity in the filter (5) is 0.5-1.2 m/s.
3. The apparatus of claim 1 for recovering suspended particles in PTA oxidation mother liquor, which is characterized in that: the side surface of the filter (5) is provided with a clear liquid diversion groove (51), and the clear liquid diversion groove (51) is connected with a clear liquid outlet pipe.
4. The apparatus of claim 1 for recovering suspended particles in PTA oxidation mother liquor, which is characterized in that: the filter (5) is a silicon carbide filter.
5. The apparatus of claim 4 for recovering suspended particles in PTA oxidation mother liquor, which is characterized in that: the filter element in the filter (5) is a 100% recrystallized silicon carbide sintered filter element.
6. The apparatus of claim 4 for recovering suspended particles in PTA oxidation mother liquor, which is characterized in that: the filtering precision of the filter (5) is 10-40 nm.
7. The apparatus of claim 1 for recovering suspended particles in PTA oxidation mother liquor, which is characterized in that: the acid liquid introduced into the acid inlet pipeline is an acetic acid solution, the concentration of the acetic acid is over 90 percent, and the temperature is over 80 ℃.
8. The use method of the device for recovering suspended particles in PTA oxidation mother liquor in accordance with any one of claims 1 to 7 is characterized in that: the method comprises the following steps:
step A, mother liquor extraction stage: opening a main mother liquor loop; the filter press (1) extracts PTA mother liquor in a mother liquor collecting tank (9) and enters a mother liquor main pipe, a mother liquor inlet adjusting valve (2) is opened, and the PTA mother liquor enters the mother liquor collecting tank (9);
step B, a filtering stage: closing the main mother liquor loop and opening the filtering branch; opening a filter inlet valve (3), closing a mother liquor inlet adjusting valve (2), introducing the PTA mother liquor into a filter (5), enabling the filter (5) to pass through a cross flow filtration mode, enabling the PTA mother liquor to flow into a mother liquor collecting tank (9) from a pipeline along the direction of a filter element of the filter (5), and enabling clear liquid to flow into a clear liquid outlet pipe from a clear liquid diversion trench; when the pressure value in the pipeline exceeds 0.25Mpa, opening a clear liquid outlet valve (6), and enabling clear liquid to enter a clear liquid collecting tank (7) through the clear liquid outlet valve (6);
step C, acid washing stage: when the pressure value in the pipeline exceeds 0.4Mpa, opening the main mother liquor loop and the pickling loop, and closing the filtering branch; opening a mother liquor inlet regulating valve (2), closing a filter inlet valve (3), a clear liquid outlet valve (6) and a filter outlet regulating valve (8), then opening an acid inlet valve (4), enabling the acidic liquid to enter a filter (5) and wash solid particles left during filtering of the membrane surface of a dissolving filter element, and fully opening the filter outlet regulating valve (8) after washing, so that the acidic liquid with the dissolved solid particles flows into a mother liquor collecting tank (9), and returns to the step A.
9. The use method of the device for recovering suspended particles in PTA oxidation mother liquor in claim 8 is characterized in that: the step B comprises the following steps:
step B1, closing the mother liquid main loop, opening the filtering branch: opening the filter inlet valve (3), fully opening the filter outlet regulating valve (8), and closing the mother liquor inlet regulating valve (2) after a period of time;
step B2, entering a filtering stage: setting a filter outlet regulating valve (8) to be in an automatic mode, and starting to filter PTA mother liquor;
step B3, clear liquid receiving stage: when the pressure value in the pipeline exceeds 0.25MPa, the clear liquid outlet valve (6) is opened, clear liquid enters the clear liquid collecting tank (7) through the clear liquid outlet valve (6), and solid suspended particles are left in the filter (5).
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