CN215799255U - Classification treatment system for caprolactam polymer slice extraction water - Google Patents
Classification treatment system for caprolactam polymer slice extraction water Download PDFInfo
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Abstract
The utility model belongs to the technical field of extraction water separation of caprolactam polymer chips, and particularly relates to a grading treatment system for extraction water of caprolactam polymer chips. The utility model provides a graded treatment system of extraction water, which comprises a filtering device, a molecular separation membrane device, an ion separation membrane device and an evaporation device which are sequentially connected through a water pipeline; a molecular separation membrane with the aperture size of 10nm-45nm is arranged in the molecular separation membrane device so as to separate the oligomer in the extraction water from the extraction water; an ion separation membrane with the aperture size of 5nm-0.1nm is arranged in the ion separation membrane device so as to separate caprolactam monomers in the extraction water from the extraction water. The extraction water grading treatment system provided by the utility model can realize effective separation of oligomers, monomers and desalted water in the extraction water, and meanwhile, the whole system has the advantages of short flow, high automation degree, low temperature and low pressure and safe operation.
Description
Technical Field
The utility model belongs to the technical field of extraction water separation of caprolactam polymer chips, and particularly relates to a grading treatment system for extraction water of caprolactam polymer chips.
Background
Nylon 6 chips are generally produced by a caprolactam hydrolysis polymerization method, wherein the caprolactam hydrolysis process comprises three stages of initiation addition, chain growth and chain balance. Wherein, the initial addition stage of caprolactam: caprolactam reacts with desalted water at a certain temperature to be hydrolyzed into omega-aminocaproic acid, the omega-aminocaproic acid and caprolactamine molecules carry out addition reaction to form short chains with a certain length, and the addition reaction of the aminocaproic acid is main at the stage because the caprolactam molecules participating in the hydrolysis reaction are few; the chain growth stage is mainly that long chain molecules are formed among short chain molecules growing in the previous stage through polycondensation, and a small amount of initiation and addition reactions are carried out in the chain growth stage, but the polycondensation reaction is mainly used; the chain balancing stage is mainly a chain exchange reaction, amide bonds on long chain molecules with different lengths are subjected to acidolysis and aminolysis under the action of terminal hydroxyl and terminal amino to cause chain exchange, hydrolysis and polycondensation are carried out in a reaction system at the same time, the molecular weight is redistributed due to the reaction in the system, and finally the system is dynamically balanced according to reaction conditions (such as temperature, moisture and the dosage of a molecular weight stabilizer) to ensure that the average molecular weight of a polymer reaches a certain value; after the caprolactam polymerization is completed, 8% -12% of low molecular weight materials are present in the reactant system, and of these low molecular weight materials, caprolactam monomer accounts for about 75%, cyclic oligomer accounts for about 25%, and of these cyclic oligomers, cyclic dimer accounts for about 70%. The melting point of the cyclic oligomer is relatively high, such as 347-348 ℃ for the cyclic dimer, and the presence of the cyclic oligomer will affect the spin-forming of the final product. Meanwhile, caprolactam monomer contained in the slices can volatilize to generate a large amount of monomer smog during processing after spinning. Therefore, the nylon 6 chips must be extracted by hot desalted water to remove caprolactam monomer and oligomer, and the obtained extraction water generally contains oligomer, caprolactam monomer and desalted water and needs to be recycled.
The existing treatment process of extracting water of caprolactam polymer slices generally removes desalted water through distillation to obtain concentrated solution, and then the concentrated solution is separated or converted and recycled to a polymerization process, and the separation or conversion process of the concentrated solution in the existing production generally comprises three processes: firstly, the German gimerak depolymerization process: rectifying 75% concentrated solution to remove residue (discharge amount is about 0.6%) and separating out oligomer, adding part of fresh caprolactam into the residual monomer, performing depolymerization reaction in a depolymerization kettle, and standing at 400 deg.C and 0.2-0.4Mpa for 2-3 hr for continuous reuse; secondly, a German high-pressure hydrolysis process, in which 75 percent of concentrated solution is subjected to cracking reaction in a hydrolysis kettle, and the concentrated solution is completely and continuously recycled after staying for 3-4 hours under the pressure of 2.5-4Mpa and the temperature of 260-; cooling 85% of the concentrated solution, feeding the cooled concentrated solution into a centrifuge, removing oligomers, and recycling the concentrated solution, wherein the operation is intermittent operation generally; fourthly, a reverse osmosis membrane is adopted to further concentrate the concentrated solution, and then the concentrated solution is recycled.
However, the process still has certain problems, the depolymerization process adopts superheated steam for heating, the energy consumption is high, the process control is more complex, the operation is complicated, and the slag is discharged under pressure, so that the process has greater safety and environmental protection risks; compared with a depolymerization process, the high-pressure hydrolysis process is simple, but needs heat-conducting oil to heat, is high in energy consumption and difficult to operate, and has safety risk; the centrifugal process is safe in process operation and reduces energy consumption, but the process needs to replace filter cloth of the centrifuge 2-4 times per shift manually, and the operation is frequent; the existing reverse osmosis membrane separation process can only realize the concentration of oligomer and polymer monomer, and cannot realize the effective separation of the oligomer, the polymer monomer and desalted water, so that the oligomer and the monomer in the extracted water cannot be effectively and reasonably utilized.
SUMMERY OF THE UTILITY MODEL
Therefore, the technical problem to be solved by the utility model is to overcome the problems that the existing process for treating and recovering the extraction water of the caprolactam polymer slices mostly adopts a method of concentrating, separating or converting for recycling, the energy consumption is high, the manual operation is complex, and the safety risk exists, while the existing process for separating the reverse osmosis membrane can reduce the energy consumption and the safety risk, but only can realize the concentration of oligomers and polymer monomers, and cannot realize the effective separation of the oligomers, the polymer monomers and desalted water, so that the oligomers and the monomers in the extraction water cannot be effectively and reasonably utilized, and further to provide a grading treatment system for the extraction water of the caprolactam polymer slices.
Therefore, the technical proposal adopted by the application is that,
a classification treatment system for extraction water of caprolactam polymer slices comprises a filtering device, a molecular separation membrane device, an ion separation membrane device and an evaporation device which are sequentially connected through a water conveying pipeline;
a molecular separation membrane with the aperture size of 10nm-45nm is arranged in the molecular separation membrane device so as to separate the oligomer in the extraction water from the extraction water;
an ion separation membrane with the aperture size of 5nm-0.1nm is arranged in the ion separation membrane device so as to separate caprolactam monomers in the extraction water from the extraction water.
Optionally, the membrane flux of the molecular separation membrane is 12-22LMH, and the membrane flux of the ionic separation membrane is 10-30 LMH.
Optionally, the molecular separation membrane is made of modified polyvinyl chloride (PVC), and the ion separation membrane is made of a polyamide composite membrane.
Optionally, the device further comprises a filter pressing device, a water inlet of the filter pressing device is connected with an oligomer aqueous solution outlet of the molecular separation membrane device, and a water outlet of the filter pressing device is connected with a water inlet of the filtering device.
Optionally, an oligomer aqueous solution storage device is arranged between the filter pressing device and the molecular separation membrane device, and the oligomer aqueous solution storage device is provided with a water inlet, a first water discharge port and a second water discharge port; the water inlet of the oligomer aqueous solution storage device is connected with the oligomer aqueous solution outlet of the molecular separation membrane device, the first water outlet of the oligomer aqueous solution storage device is connected with the water inlet of the filter pressing device, and the second water outlet of the oligomer aqueous solution storage device is connected with the water inlet of the molecular separation membrane device.
Optionally, the method further comprises the step of,
the extraction water storage device is arranged between the filtering device and the molecular separation membrane device and is used for storing the extraction water obtained after filtering;
the caprolactam monomer aqueous solution storage device is arranged between the molecular separation membrane device and the ion separation membrane device and is used for storing caprolactam monomer aqueous solution discharged from the molecular separation membrane device;
and the caprolactam monomer concentrated solution storage device is arranged between the ion separation membrane device and the evaporation device and is used for storing the caprolactam monomer concentrated solution discharged from the ion separation membrane device.
Optionally, the filter pressing device is also provided with a solid oligomer discharge port;
the filtering device is also provided with a solid impurity discharge port;
the ion separation membrane device also has a desalted water discharge port.
Optionally, the evaporation device is an MVR evaporator.
Optionally, the caprolactam polymer chip extraction water contains oligomer, caprolactam monomer and desalted water.
The technical scheme of the utility model has the following advantages:
1. the utility model provides a classification treatment system of caprolactam polymer chip extract water, which is different from the prior process of concentrating and separating extract water in the prior process of extract water treatment, firstly, the extract water passes through a filtering device to remove solid impurities in the extract water, then the filtered extract water is introduced into a molecular separation membrane device with a specific pore diameter to separate oligomers in the extract water from the extract water to obtain an aqueous solution of the oligomers and extract water containing caprolactam monomers and desalted water, the extract water containing the caprolactam monomers and the desalted water is introduced into an ion separation membrane device with a specific pore diameter to realize the separation of the desalted water and the caprolactam monomers to obtain desalted water and a concentrated solution of the caprolactam monomers, thereby realizing the effective separation of the oligomers, the monomers and the desalted water, the concentrated solution of the caprolactam monomers is introduced into an evaporation device to evaporate water in the concentrated solution of the caprolactam monomers, caprolactam monomer is obtained, and desalted water obtained by separation can be reused in the extraction process.
The classification treatment system for the caprolactam polymer slice extraction water provided by the utility model adopts a mode of separating first and then concentrating to treat the nylon 6 slice extraction water, and tests show that the molecular separation membrane and the ion separation membrane with specific pore diameters are suitable for separating the extraction water, the caprolactam monomer concentration can be improved by more than one time to reach 20-30 wt%, and the desalted water can be reduced by more than 50%.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a system for fractionating caprolactam polymer chip extract water according to the present invention.
Wherein the reference numerals are represented as:
1. a filtration device; 2. an extraction water storage device; 3. a molecular separation membrane device; 4. a caprolactam monomer aqueous solution storage device; 5. an ion separation membrane device; 6. a caprolactam monomer concentrated solution storage device; 7. an evaporation device; 8. an oligomer aqueous solution storage device; 9. a filter pressing device; 10. a solid oligomer storage unit; 11. a solid impurity storage device; 12. desalted water
And a storage device.
Detailed Description
The technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
As shown in fig. 1, the present embodiment provides a staged treatment system for extraction water of caprolactam polymer chip, which comprises a filtering device 1, a molecular separation membrane device 3, an ion separation membrane device 5 and an evaporation device 7, which are connected in sequence through a water pipeline;
a molecular separation membrane with the aperture size of 10nm-45nm is arranged in the molecular separation membrane device 3 so as to separate the oligomer in the extraction water from the extraction water;
an ion separation membrane with the aperture size of 5nm-0.1nm is arranged in the ion separation membrane device 5 so as to separate caprolactam monomers in the extraction water from the extraction water.
In an alternative embodiment, the membrane flux of the molecular separation membrane is 12-22LMH, and optionally, the membrane flux of the molecular separation membrane is 15LMH (L/(m))2H)); the membrane flux of the ion separation membrane is 10-30LMH, and optionally, the membrane flux of the ion separation membrane is 20LMH (L/(m) m2·h))。
In an alternative embodiment, the filter device 1 is a filter, and the filter device 1 has a water inlet, a water outlet and a solid impurity discharge port.
In an alternative embodiment, a solid impurity storage device 11 is further included, and the feed inlet of the solid impurities is connected with the solid impurities discharge outlet of the filtering device 1.
The molecular separation membrane device 3 and the ion separation membrane device 5 are both of the existing structures, and the molecular separation membrane and the ion separation membrane can be obtained by a commercially available or existing preparation method. In an optional embodiment, the molecular separation membrane is a hollow fiber ultrafiltration membrane, and the ionic separation membrane is a reverse osmosis membrane. In an optional embodiment, the molecular separation membrane is made of modified polyvinyl chloride (PVC), and the ion separation membrane is made of a polyamide composite membrane; the molecular separation membrane is purchased from Heideneng, USA, model HUF-90; ion separation membranes were purchased from the heidenerg model, PROC10, usa.
In an optional embodiment, the device further comprises a filter pressing device 9, wherein the filter pressing device 9 is provided with a water inlet, a water outlet and a solid oligomer discharge port, optionally, the filter pressing device 9 is a filter press, the water inlet of the filter pressing device 9 is connected with the oligomer aqueous solution discharge port of the molecular separation membrane device 3, and the water outlet of the filter pressing device 9 is connected with the water inlet of the filtering device 1.
In an alternative embodiment, a solid oligomer storage device 10 is further included, and the feed inlet of the solid oligomer storage device 10 is connected with the solid oligomer discharge outlet of the filter press device 9.
In an alternative embodiment, an oligomer aqueous solution storage device 8 is arranged between the filter pressing device 9 and the molecular separation membrane device 3, and the oligomer aqueous solution storage device 8 is provided with a water inlet, a first water discharge opening and a second water discharge opening; the water inlet of the oligomer aqueous solution storage device 8 is connected with the oligomer aqueous solution outlet of the molecular separation membrane device 3, the first water outlet of the oligomer aqueous solution storage device 8 is connected with the water inlet of the filter pressing device 9, and the second water outlet of the oligomer aqueous solution storage device 8 is connected with the water inlet of the molecular separation membrane device 3.
In an alternative embodiment, the method further comprises,
the extraction water storage device 2 is arranged between the filtering device 1 and the molecular separation membrane device 3 and is used for storing the extraction water obtained after filtering; optionally, the extraction water storage device 2 is an extraction water storage tank;
the caprolactam monomer aqueous solution storage device 4 is arranged between the molecular separation membrane device 3 and the ion separation membrane device 5 and is used for storing caprolactam monomer aqueous solution discharged from the molecular separation membrane device 3; optionally, the caprolactam monomer aqueous solution storage device 4 is a caprolactam monomer aqueous solution storage tank;
and the caprolactam monomer concentrated solution storage device 6 is arranged between the ion separation membrane device 5 and the evaporation device 7 and is used for storing the caprolactam monomer concentrated solution discharged from the ion separation membrane device 5. Optionally, the caprolactam monomer concentrated solution storage device 6 is a caprolactam monomer concentrated solution storage tank.
In an alternative embodiment, the ion separation membrane device 5 also has a desalted water discharge port.
In an optional embodiment, the ion separation membrane device further comprises a desalted water storage device 12, wherein the desalted water storage device 12 is an optional desalted water storage tank, and a water inlet of the desalted water storage device 12 is connected with a desalted water outlet of the ion separation membrane device 5.
In an alternative embodiment, the evaporation device 7 is an MVR evaporator.
In an alternative embodiment, the caprolactam polymer chip extract water comprises oligomers, caprolactam monomers and desalted water.
In the utility model, because the low polymer is formed by polycondensing caprolactam monomers, the molecular mass of the low polymer is far larger than that of the caprolactam monomers and water, a molecular separation membrane with the membrane aperture of 10-45 nm is selected to firstly separate the low polymer in the extraction water. The molecular separation membrane is a nano-scale microporous filter membrane, desalted water and caprolactam monomers flow out through the molecular separation membrane under the drive of pressure, and oligomers are intercepted by the molecular separation membrane, so that the separation of the oligomers, the desalted water and the caprolactam monomers is realized. Through experimental tests, the driving pressure of the extraction water is controlled to be 1.0-1.5Mpa, and the flux of the molecular separation membrane is controlled to be about 12-22 LMH.
Further, the caprolactam monomer is separated from the extract water containing the caprolactam monomer and desalted water by selecting an ion separation membrane for separation, wherein the ion separation membrane is a hydrophilic reverse osmosis membrane, when organic matters in the mixed solution contact with the surface of the membrane, the surface tension of the membrane is reduced, and when water contacts with the surface of the membrane, the surface tension of the membrane is increased. Because the ion separation membrane is a hydrophilic reverse osmosis membrane, when the mixed solution is contacted with the membrane surface, the membrane surface can produce negative adsorption to organic matters, and can produce positive adsorption to water, so that after the mixed solution is contacted with the membrane surface, a pure water layer with a certain thickness can be formed on a contact interface, under a certain pressure, the pure water layer can enter the membrane surface, and the organic matters in the solution can be intercepted outside the membrane, so that the water and the caprolactam monomer can be effectively separated. Under the drive of pressure, the desalted water and the caprolactam monomer are separated, and through experimental tests, the drive pressure is controlled to be 2.0-3.0Mpa, and the flow rate of desalted water and the flow rate of caprolactam monomer are controlled to be 0.4-0.55.
In the utility model, caprolactam polymer chip extract water from a chip extraction process (the concentration of monomers and oligomers in the extract water is 10 wt%, the mass ratio of the monomers to the oligomers is 3: 1, the temperature is 30-40 ℃) is pressurized by a pump and passes through a filtering device 1, solid impurities such as chip powder and the like in the extract water are filtered, the extract water enters an extract water storage device 2, then the extract water is pressurized to 1.0-1.5Mpa by the pump and enters a molecular separation membrane device 3, an aqueous solution containing a large amount of oligomers and extract water containing caprolactam monomers and desalted water (the concentration of the monomers in the extract water is 6-9 wt%) are separated, the aqueous solution of the oligomers enters an aqueous solution storage device 8, is pressurized by the pump and circulated back to the molecular separation membrane device 3 for continuous concentration until the concentration of the oligomers is 20-25 wt%, and then enters a filter pressing device 9, and filtering the clear liquid after pressure filtration in a filtering device 1, and selling the solid oligomer obtained after pressure filtration.
The extraction water containing caprolactam monomer and desalted water enters a caprolactam monomer aqueous solution storage device 4, is pressurized to 2.0-3.0Mpa by a pump and then enters an ion separation membrane device 5, desalted water and caprolactam monomer concentrated solution with the mass fraction of about 20 percent are obtained by separation, and desalted water enters a desalted water storage device 12 and is recycled to the extraction process; and (3) conveying the caprolactam monomer concentrated solution into a caprolactam monomer concentrated solution storage device 6, conveying the caprolactam monomer concentrated solution to an MVR evaporator through a pump, and evaporating to remove moisture in the caprolactam monomer concentrated solution to obtain a caprolactam monomer, wherein the caprolactam monomer can be used as a polymerization raw material of nylon 6.
Example 2
The embodiment provides a classification treatment method of caprolactam polymer chip extract water, which comprises the following steps:
the extract water from the caprolactam polymer chip from the chip extraction step (concentration of monomer and oligomer in the extract water is 10 wt%, mass ratio of monomer and oligomer is 3: 1, temperature is 35 ℃) was pumped at 10m3The flow rate of/h passes through the filtering device 1, solid impurities such as slice powder and the like in the extraction water are filtered, and then the extraction water enters the extraction water storage device 2, butThen pressurizing to 1.0Mpa by pump to 10m3The flow rate/h is fed into a molecular separation membrane unit 3, and an aqueous solution containing a large amount of oligomers and an extract water containing caprolactam monomer and desalted water (the monomer concentration in the extract water is 8.3 wt%) are separated, and the oligomer aqueous solution is 1m3The flow of the solution per hour enters an oligomer aqueous solution storage device 8, is pressurized by a pump and circularly returns to the molecular separation membrane device 3 to be continuously concentrated until the concentration of the oligomer is 23 wt%, and then enters a filter pressing device 9, clear liquid after filter pressing enters a filter device 1 to be filtered, and solid oligomer obtained after filter pressing is sold.
The extraction water containing caprolactam monomer and desalted water enters a caprolactam monomer aqueous solution storage device 4, is pressurized to 2.0Mpa by a pump and then is 9m3The flow rate of the desalted water is fed into an ion separation membrane device 5, the desalted water and the caprolactam monomer concentrated solution with the mass fraction of 20 percent are obtained by separation, and the desalted water is 6.6m3The flow of the water/h enters a desalted water storage device 12 and is recycled to the extraction procedure; the caprolactam monomer concentrated solution is 2.4m3The flow of the caprolactam monomer per hour enters a caprolactam monomer concentrated solution storage device 6, the caprolactam monomer concentrated solution is conveyed to an MVR evaporator by a pump, the moisture in the caprolactam monomer concentrated solution is removed by evaporation, and the caprolactam monomer is obtained and can be used as a polymerization raw material of nylon 6.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the utility model.
Claims (8)
1. A classification treatment system for extraction water of caprolactam polymer slices is characterized by comprising a filtering device, a molecular separation membrane device, an ion separation membrane device and an evaporation device which are sequentially connected through a water conveying pipeline;
a molecular separation membrane with the aperture size of 10nm-45nm is arranged in the molecular separation membrane device;
an ion separation membrane with the aperture size of 5nm-0.1nm is arranged in the ion separation membrane device.
2. The system for fractionating caprolactam polymer chip extract water according to claim 1, wherein said molecular separation membrane has a membrane flux of 12-22LMH and said ionic separation membrane has a membrane flux of 10-30 LMH.
3. The system for fractionating caprolactam polymer chip extract water according to claim 1 or 2, wherein the molecular separation membrane is made of modified polyvinyl chloride, and the ionic separation membrane is made of a polyamide composite membrane.
4. The system for the fractional treatment of caprolactam polymer chip extract water of claim 3, further comprising a filter press device, wherein the water inlet of the filter press device is connected with the oligomer aqueous solution outlet of the molecular separation membrane device, and the water outlet of the filter press device is connected with the water inlet of the filter device.
5. The system for the fractional treatment of caprolactam polymer chip extract water of claim 4, wherein an oligomer aqueous solution storage device is arranged between the pressure filtration device and the molecular separation membrane device, and the oligomer aqueous solution storage device is provided with a water inlet, a first water discharge opening and a second water discharge opening; the water inlet of the oligomer aqueous solution storage device is connected with the oligomer aqueous solution outlet of the molecular separation membrane device, the first water outlet of the oligomer aqueous solution storage device is connected with the water inlet of the filter pressing device, and the second water outlet of the oligomer aqueous solution storage device is connected with the water inlet of the molecular separation membrane device.
6. The system for fractionating a caprolactam polymer chip extract water according to claim 1, further comprising,
the extraction water storage device is arranged between the filtering device and the molecular separation membrane device and is used for storing the extraction water obtained after filtering;
the caprolactam monomer aqueous solution storage device is arranged between the molecular separation membrane device and the ion separation membrane device and is used for storing caprolactam monomer aqueous solution discharged from the molecular separation membrane device;
and the caprolactam monomer concentrated solution storage device is arranged between the ion separation membrane device and the evaporation device and is used for storing the caprolactam monomer concentrated solution discharged from the ion separation membrane device.
7. The system for fractionation of caprolactam polymer chip extract water according to claim 5, wherein said pressure filtration device further has a solid oligomer discharge port;
the filtering device is also provided with a solid impurity discharge port;
the ion separation membrane device also has a desalted water discharge port.
8. The system for fractionating caprolactam polymer chip extract water according to claim 1, wherein said evaporation apparatus is an MVR evaporator.
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