CN103913527A - On-line sampling and analysis system and method of aromatization process - Google Patents
On-line sampling and analysis system and method of aromatization process Download PDFInfo
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Abstract
The invention discloses an on-line sampling and analysis system and method of an aromatization process. The system comprises a material flow extraction device connected with an outlet of a reactor or a middle device, and a gas-solid separation device, a filter and an on-line analysis system which are successively connected with the material flow extraction device, wherein the material flow extraction device, the gas-solid separation device and the filter are all arranged in a heat-insulation system. The method comprises the following steps: 1, extracting an aromatization material from the outlet of the reactor or the middle device through the material flow extraction device; 2, carrying out heat preservation on equipment and a pipeline from the material flow extraction device to en entrance of the on-line analysis system; 3, removing a catalyst carried by the extracting material; 4, further removing catalyst fine particles in the material; and 5, feeding the material into the on-line analysis system, and analyzing components of the material. The system and the method provided by the invention can solve the problems that in an on-line sampling process of an aromatization device in the prior art, an aromatization product composition is complicated, solid particulate matters carried by the product and heavy constituent liquidation of the product can cause the large fluctuation range and frequency of analysis data, and a chromatography can not continuously stably operate.
Description
Technical field
The present invention relates to aromatization process technical field, particularly a kind of online sampling of aromatization process and the System and method for of analysis.
Background technology
Aromatic hydrocarbons is one of most important Essential Chemistry product, and in traditional chemical industry route, aromatic hydrocarbons is mainly that petroleum refining and coal carbonization processing obtain.Compared with coal carbonization technology path, the aromatic hydrocarbons purity that petroleum path obtains is high, is suitable for preparing various high-quality chemicals.The aromatic hydrocarbons that coal (destructive distillation) route obtains is owing to containing thiophene-based impurity, and quality is relatively low, and application is limited to, along with petroleum resources worsening shortages, the supply of aromatic hydrocarbons is nervous trend, holds at high price, greatly improve the manufacturing cost of subsequent chemicals, its sale is affected.The raw material such as methyl alcohol, dimethyl ether can be from the gasification of coal, rock gas, living beings or shale gas etc., methyl alcohol synthetic and methanol dehydration process be prepared, the amount of having is large, the advantage that cost is low, therefore the research of the aromatization process such as methyl alcohol and C2-C6 has received increasing concern in recent years.
For the industrial reactor of aromizing, its major control target is to control the selectivity of reaction depth, turnout and product, the accurate on-line analysis Real-time Feedback of in operation main dependent reaction device outlet process gas, off-line sample analysis can not meet modernization industry device control needs.On-line chromatograph analysis has the strong feature of continuity that measurement range is wide, analysis is accurate, the cycle is short, automaticity is high, analyze data, in some petrochemical equipments, existing on-line chromatograph is analyzed for the key component in product, the example that the data feedback DCS system obtaining is controlled for advanced person.
But because the process gas temperature of aromizing is high, water cut is large, composition is complicated, its boiling point is from subzero more than 250 degree to several Baidu above freezing, simultaneously in process gas, carry a certain amount of catalyst granules secretly and may cause the obstruction of whole sampling analytical system, moisture and heavy arene can pollute on-line chromatograph simultaneously, cause shorten the serviceable life of on-line chromatograph, accuracy declines, and in these sampling craft materials, solid impurity and heavy constituent material inevitably will stop up process line, analysis data fluctuations scope and frequency that while also may cause because the heavy constituent in product liquefies are large, chromatogram cannot continuous and steady operation problem, cannot provide basic data accurately and timely for aromatization of methanol industrial reaction apparatus.
Summary of the invention
The problem existing in order to solve prior art, the object of the present invention is to provide a kind of online sampling of aromatization process and the System and method for of analysis, in the online sampling process of aromizing device that solution prior art exists, exist aromizing product composition complicated, the liquefaction of entrained solids particle and heavy constituent cause analyzing data fluctuations scope and frequency large, the problem that chromatogram cannot continuous and steady operation.
In order to achieve the above object, technical scheme of the present invention is:
A kind of online sampling of aromatization process and the system of analysis, comprise the logistics ejector 2 being connected with the outlet of reactor or middle device 1, the gas-solid separating device 3, filtrator 4 and the on-line analysis system 5 that are connected successively with logistics ejector 2, described logistics ejector 2, gas-solid separating device 3 and filter 4 are all placed in heat-insulation system.
Described on-line analysis system 5 is by the automatic six-way valve of two series connection, the permanent gases analysis systems such as hydrogen, carbon monoxide, carbon dioxide, hydro carbons C
1-C
4hydrocarbon analysis system and oil phase product are C
5-C
7non-aromatics and aromatic hydrocarbons and methyl alcohol analytic system composition.
The online sampling of system described above and the method for analyzing, comprise the steps:
Step 1: draw logistics: draw one aromizing product material from the outlet of reactor or middle device 1 by logistics ejector 2;
Step 2: system insulation: be incubated to the equipment and the pipeline that enter on-line analysis system 5 from logistics ejector 2, guarantee the not condensation in gas solid separation and filter process of aromizing product material;
Step 3: gas solid separation: remove entrained catalyzer in the aromizing product material that step 1 draws;
Step 4: filter: further remove the catalyst fines in aromizing product material after gas solid separation;
Step 5: on-line analysis: the aromizing product material after filtering is passed into on-line analysis system 5 and analyzes, analyze the composition of permanent gases wherein, methyl alcohol, water, aromatic hydrocarbon product.
The aromizing product material of drawing described in step 1 is aromatization of methanol or C
2-C
6the product of aromatization of hydrocarbons, it specifically consists of hydrogen, C
1-C
4hydro carbons and C
5-C
10non-aromatics and aromatic hydrocarbons, and water, methyl alcohol, carbon monoxide, carbon dioxide.
Described in step 2, the temperature of system insulation is 180-300 ℃.
Compared to the prior art, advantage of the present invention is as follows:
The present invention is for aromatization of methanol or C
2-C
6the on-line analysis sample of aromatizing reaction of hydrocarbons device is processed, remove the catalyst granules of gaseous products, and according to the specific intermediate condensation that provides process insulation to prevent product of material, and adopt the chromatogram sampling system that adapts, rational material is offered to chromatogram, analyze accurately the composition of gas phase in aromatization of methanol product, water, oil phase, realize the method for long-term, the stable operation of on-line analysis.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of the online sampling of the present invention and analytic system.
Fig. 2 is the process flow diagram of invention on-line analysis system.
In Fig. 2: 6-the first six-way valve injector, 7-the first quantity tube, 8-the first injection port, 9-first fills pre-column, 10-the first chromatogram column system, 11-the one FID chromatographic detector, 12-the second chromatogram column system, 13-the 2nd FID chromatographic detector, 14-the second six-way valve injector, 15-the second quantity tube, 16-emptying, 17-the second injection port, 18-second fills pre-column, 19-the 3rd chromatogram column system, 20-TCD chromatographic detector, 21-the first carrier gas inlet, 22-the second carrier gas inlet, 23-blowback is emptying.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described in detail.
As shown in Figure 1, the online sampling of a kind of aromatization process of the present invention and the system of analysis, comprise the logistics ejector 2 being connected with the outlet of reactor or middle device 1, the gas-solid separating device 3, filtrator 4 and the on-line analysis system 5 that are connected successively with logistics ejector 2, described logistics ejector 2, gas-solid separating device 3 and filter 4 are all placed in heat-insulation system.Described logistics ejector 2 is for drawing product from the outlet of reactor or middle device 1, described gas-solid separating device 3 is for removing the catalyst granules of gas product, described filtrator 4 is for further removing the catalyst granules of gas product, described heat-insulation system is used for heating whole system and prevents gas product condensation during the course, and described on-line analysis system 5 is for the composition of analytic product gas.
As shown in Figure 1, the online sampling of system of the present invention and the method for analyzing, comprise the steps:
Step 1: draw logistics: draw one aromizing product material from the outlet of reactor or middle device 1 by logistics ejector 2;
Step 2: system insulation: be incubated to the equipment and the pipeline that enter on-line analysis system 5 from logistics ejector 2, guarantee the not condensation in gas solid separation and filter process of aromizing product material;
Step 3: gas solid separation: remove entrained catalyzer in the aromizing product material that step 1 draws;
Step 4: filter: further remove the catalyst fines in aromizing product material after gas solid separation;
Step 5: on-line analysis: the aromizing product material after filtering is passed into on-line analysis system 5 and analyzes, analyze the composition of permanent gases wherein, methyl alcohol, water, aromatic hydrocarbon product.
Embodiment 1:
First open the heating arrangement of on-line analysis system, maintaining intrasystem temperature is 180 ℃.The product of aromatization of methanol reaction is incorporated into online sampler from aromatization of methanol reactor outlet by logistics ejector 2, first remove through a gas-solid separating device 3 most of catalyst granules of carrying secretly in gas product, remove the fine particle in gaseous products through an accurate filter again, enter on-line analysis system 5.Wherein, the chromatographic column of on-line analysis system and operating conditions are as table 1.
First, gas product enters in the first six-way valve injector 6, in the first quantity tube 7, retain, switching the first six-way valve injector 6 makes a certain amount of sample gas enter the first filling pre-column 9 by the first injection port 8, then entering the first chromatogram column system 10 separation of C 1-C4 hydro carbons enters a FID chromatographic detector 11 and detects, the analysis of C1-C4 hydro carbons to be completed, change pressure makes to be retained in the 2nd FID chromatographic detector 13 that enters that sample in the first filling pre-column 9 enters the second chromatogram column system 12 separation of methanol and C5-C7 non-aromatics and aromatic hydrocarbons and analyzes.
On the other hand, gas product enters in the second six-way valve injector 14, in the second quantity tube 15, retain, switching the second six-way valve injector 14 makes a certain amount of sample gas first enter the second filling pre-column 18 by the second injection port 17, in the 3rd chromatogram column system 19, separate and in TCD chromatographic detector 20, analyze the permanent gases such as hydrogen, carbon monoxide, carbon dioxide, after to be analyzed completing, other gas product blowbacks being gone out to chromatographic column.
Adopt said method on-line chromatograph method to analyze continuously the product of aromatization of methanol commercial plant, continuous 5 automatic sampling analysis results within 8 hours, carry out relevant treatment and calculate result and off-line analysis result are compared.Result shows that the running of this on-line analysis system is stable, and testing result and off-line analysis result exist good consistance, as shown in table 2.
Table 1 on-line analysis system chromatographic column and analysis condition
The result of the analysis aromatization of methanol reaction of table 2 on-line analysis system
| Sequence number | 1 | 2 | 3 | Off-line sampling |
| Carbon monoxide (wt%) | 0.23 | 0.22 | 0.22 | 0.23 |
| Carbon dioxide (wt%) | 0.45 | 0.44 | 0.44 | 0.45 |
| Hydrogen (wt%) | 1.04 | 1.05 | 1.05 | 1.04 |
| Methane (wt%) | 1.91 | 1.92 | 1.92 | 1.91 |
| Ethene (wt%) | 1.54 | 1.55 | 1.55 | 1.54 |
| Ethane (wt%) | 1.75 | 1.73 | 1.73 | 1.75 |
| Propylene (wt%) | 19.82 | 19.81 | 19.81 | 19.82 |
| Propane (wt%) | 2.01 | 1.99 | 1.99 | 2.01 |
| Butylene (wt%) | 1.15 | 1.13 | 1.13 | 1.15 |
| Butane (wt%) | 8.98 | 9 | 9 | 8.98 |
| Amylene (wt%) | 2.04 | 2.04 | 2.04 | 2.04 |
| Pentane (wt%) | 0.21 | 0.21 | 0.21 | 0.21 |
| Hexene (wt%) | 0.21 | 0.21 | 0.21 | 0.21 |
| Hexane (wt%) | 1.13 | 1.13 | 1.13 | 1.13 |
| Benzene (wt%) | 0.92 | 0.92 | 0.92 | 0.92 |
| Toluene (wt%) | 11.31 | 11.32 | 11.32 | 11.31 |
| Ethylbenzene (wt%) | 0.43 | 0.43 | 0.43 | 0.43 |
| Dimethylbenzene (wt%) | 32.54 | 32.56 | 32.56 | 32.54 |
| Trimethylbenzene above (wt%) | 11.72 | 11.73 | 11.73 | 11.72 |
| Coke (wt%) | 0.62 | 0.63 | 0.63 | 0.62 |
Embodiment 2
First open the heating arrangement of on-line analysis system, maintaining intrasystem temperature is 300 ℃.The product of propylene reaction is incorporated into online sampler from aromatization of methanol reactor outlet by logistics ejector 2, first remove through a gas-solid separating device 3 most of catalyst granules of carrying secretly in gas product, removing the fine particle in gaseous products through an accurate filter, enter on-line analysis system 5.Wherein, the chromatographic column of on-line analysis system 5 and operating conditions are with table 1.
First, gas product enters in the first six-way valve injector 6, in the first quantity tube 7, retain, switching the first six-way valve injector 6 makes a certain amount of sample gas enter the first filling pre-column 9 by the first injection port 8, then entering the first chromatogram column system 10 separation of C 1-C4 hydro carbons enters a FID chromatographic detector 11 and detects, the analysis of C1-C4 hydro carbons to be completed, change pressure makes to be retained in the 2nd FID chromatographic detector 13 that enters that sample in the first filling pre-column 9 enters the second chromatogram column system 12 separation of methanol and C5-C7 non-aromatics and aromatic hydrocarbons and analyzes.
On the other hand, gas product enters in the second six-way valve injector 14, in the second quantity tube 15, retain, switching the second six-way valve injector 14 makes a certain amount of sample gas first enter the second filling pre-column 18 by the second injection port 17, in the 3rd chromatogram column system 19, separate and in TCD chromatographic detector 20, analyze the permanent gases such as hydrogen, carbon monoxide, carbon dioxide, after to be analyzed completing, other gas product blowbacks being gone out to chromatographic column.
Adopt said method on-line chromatograph method to carry out analyzing continuously the product of light-hydrocarbon aromatized commercial plant, continuous 5 automatic sampling analysis results within 8 hours, carry out relevant treatment and calculate result and off-line analysis result are compared.Result shows that this on-line analysis system dress turns stable, and testing result and off-line analysis result exist good consistance, as shown in table 3.
The result of the analysis propylene aromatization of table 3 on-line analysis system
Embodiment 3
First open the heating arrangement of on-line analysis system, maintaining intrasystem temperature is 250 ℃.The product of propane aromatization reaction is incorporated into online sampler from aromatization of methanol reactor outlet by logistics ejector 2, first remove through a gas-solid separating device 3 most of catalyst granules of carrying secretly in gas product, removing the fine particle in gaseous products through an accurate filter, enter on-line analysis system 5.Wherein, the chromatographic column of on-line analysis system and operating conditions are with table 1.
First, gas product enters in the first six-way valve injector 6, in the first quantity tube 7, retain, switching the first six-way valve injector 6 makes a certain amount of sample gas enter the first filling pre-column 9 by the first injection port 8, then entering the first chromatogram column system 10 separation of C 1-C4 hydro carbons enters a FID chromatographic detector 11 and detects, the analysis of C1-C4 hydro carbons to be completed, change pressure makes to be retained in the 2nd FID chromatographic detector 13 that enters that sample in the first filling pre-column 9 enters the second chromatogram column system 12 separation of methanol and C5-C7 non-aromatics and aromatic hydrocarbons and analyzes.
On the other hand, gas product enters in the second six-way valve injector 14, in the second quantity tube 15, retain, switching the second six-way valve injector 14 makes a certain amount of sample gas first enter the second filling pre-column 18 by the second injection port 17, in the 3rd chromatogram column system 19, separate and in TCD chromatographic detector 20, analyze the permanent gases such as hydrogen, carbon monoxide, carbon dioxide, after to be analyzed completing, other gas product blowbacks being gone out to chromatographic column.
Adopt said method on-line chromatograph method to carry out analyzing continuously the product of light-hydrocarbon aromatized commercial plant, continuous 5 automatic sampling analysis results within 8 hours, carry out relevant treatment and calculate result and off-line analysis result are compared.Result shows that this on-line analysis system dress turns stable, and testing result and off-line analysis result exist good consistance, as shown in table 4.
The result of the analysis aromatization of methanol reaction of table 4 on-line analysis system
Embodiment 4
First open the heating arrangement of on-line analysis system, maintaining intrasystem temperature is 280 ℃.The product of butane aromatization is incorporated into online sampler from aromatization of methanol reactor outlet by logistics ejector 2, first remove through a gas-solid separating device 3 most of catalyst granules of carrying secretly in gas product, removing the fine particle in gaseous products through an accurate filter, enter on-line analysis system 5.Wherein, the chromatographic column of on-line analysis system and operating conditions are with table 1.
First, gas product enters in the first six-way valve injector 6, in the first quantity tube 7, retain, switching the first six-way valve injector 6 makes a certain amount of sample gas enter the first filling pre-column 9 by the first injection port 8, then entering the first chromatogram column system 10 separation of C 1-C4 hydro carbons enters a FID chromatographic detector 11 and detects, the analysis of C1-C4 hydro carbons to be completed, change pressure makes to be retained in the 2nd FID chromatographic detector 13 that enters that sample in the first filling pre-column 9 enters the second chromatogram column system 12 separation of methanol and C5-C7 non-aromatics and aromatic hydrocarbons and analyzes.
On the other hand, gas product enters in the second six-way valve injector 14, in the second quantity tube 15, retain, switching the second six-way valve injector 14 makes a certain amount of sample gas first enter the second filling pre-column 18 by the second injection port 17, in the 3rd chromatogram column system 19, separate and in TCD chromatographic detector 20, analyze the permanent gases such as hydrogen, carbon monoxide, carbon dioxide, after to be analyzed completing, other gas product blowbacks being gone out to chromatographic column.
Adopt said method on-line chromatograph method to analyze continuously the product of butylene aromizing commercial plant, continuous 5 automatic sampling analysis results within 8 hours, carry out relevant treatment and calculate result and off-line analysis result are compared.Result shows that this on-line analysis system dress turns stable, and testing result and off-line analysis result exist good consistance, as shown in table 5.
The result of the analysis butane aromatization of table 5 on-line analysis system
Embodiment 5
First open the heating arrangement of on-line analysis system, maintaining intrasystem temperature is 220 ℃.The raw material of this process is hydrocarbon mixture, and it consists of in table 6.
The product of hydrocarbon mixture aromatization is incorporated into online sampler from aromatization of methanol reactor outlet by logistics ejector 2, first remove through a gas-solid separating device 3 most of catalyst granules of carrying secretly in gas product, removing the fine particle in gaseous products through an accurate filter, enter on-line analysis system 5.Wherein, the chromatographic column of on-line analysis system and operating conditions are with table 1.
First, gas product enters in the first six-way valve injector 6, in the first quantity tube 7, retain, switching the first six-way valve injector 6 makes a certain amount of sample gas enter the first filling pre-column 9 by the first injection port 8, then entering the first chromatogram column system 10 separation of C 1-C4 hydro carbons enters a FID chromatographic detector 11 and detects, the analysis of C1-C4 hydro carbons to be completed, change pressure makes to be retained in the 2nd FID chromatographic detector 13 that enters that sample in the first filling pre-column 9 enters the second chromatogram column system 12 separation of methanol and C5-C7 non-aromatics and aromatic hydrocarbons and analyzes.
On the other hand, gas product enters in the second six-way valve injector 14, in the second quantity tube 15, retain, switching the second six-way valve injector 14 makes a certain amount of sample gas first enter the second filling pre-column 18 by the second injection port 17, in the 3rd chromatogram column system 19, separate and in TCD chromatographic detector 20, analyze the permanent gases such as hydrogen, carbon monoxide, carbon dioxide, after to be analyzed completing, other gas product blowbacks being gone out to chromatographic column.
Adopt said method on-line chromatograph method to analyze continuously the product of butylene aromizing commercial plant, continuous 5 automatic sampling analysis results within 8 hours, carry out relevant treatment and calculate result and off-line analysis result are compared.Result shows that this on-line analysis system dress turns stable, and testing result and off-line analysis result exist good consistance, as shown in table 7.
The raw material composition of table 6 hydrocarbon mixture aromizing
| Ethene (wt%) | 7.9 |
| Ethane (wt%) | 7.4 |
| Propylene (wt%) | 10.3 |
| Propane (wt%) | 31.3 |
| Butylene (wt%) | 10.5 |
| Butane (wt%) | 30.5 |
| Amylene (wt%) | 2.1 |
The result of the analysis aromatization of methanol reaction of table 7 on-line analysis system
| Sequence number | 1 | 2 | 3 | Off-line sampling |
| Carbon monoxide (wt%) | 0.00 | 0.00 | 0.00 | 0.00 |
| Carbon dioxide (wt%) | 0.00 | 0.00 | 0.00 | 0.00 |
| Hydrogen (wt%) | 1.16 | 1.16 | 1.16 | 1.16 |
| Methane (wt%) | 7.31 | 7.30 | 7.30 | 7.30 |
| Ethene (wt%) | 2.39 | 2.39 | 2.39 | 2.39 |
| Ethane (wt%) | 11.05 | 11.04 | 11.04 | 11.05 |
| Propylene (wt%) | 2.91 | 2.92 | 2.91 | 2.91 |
| Propane (wt%) | 35.36 | 35.36 | 35.36 | 35.36 |
| Butylene (wt%) | 1.07 | 1.07 | 1.07 | 1.07 |
| Butane (wt%) | 9.50 | 9.50 | 9.50 | 9.50 |
| Amylene (wt%) | 1.53 | 1.53 | 1.53 | 1.53 |
| Pentane (wt%) | 0.15 | 0.15 | 0.15 | 0.15 |
| Hexene (wt%) | 0.34 | 0.34 | 0.34 | 0.34 |
| Hexane (wt%) | 0.90 | 0.90 | 0.90 | 0.90 |
| Benzene (wt%) | 4.18 | 4.18 | 4.18 | 4.18 |
| Toluene (wt%) | 10.36 | 10.36 | 10.36 | 10.36 |
| Ethylbenzene (wt%) | 0.73 | 0.73 | 0.73 | 0.73 |
| Dimethylbenzene (wt%) | 5.78 | 5.77 | 5.78 | 5.78 |
| Trimethylbenzene above (wt%) | 4.07 | 4.08 | 4.08 | 4.08 |
| Coke (wt%) | 1.20 | 1.21 | 1.21 | 1.21 |
Claims (5)
1. the online sampling of an aromatization process and the system of analysis, it is characterized in that: comprise the logistics ejector (2) being connected with the outlet of reactor or middle device (1), the gas-solid separating device (3), filtrator (4) and the on-line analysis system (5) that are connected successively with logistics ejector (2), described logistics ejector (2), gas-solid separating device (3) and filter (4) are all placed in heat-insulation system.
2. the online sampling of a kind of aromatization process according to claim 1 and the system of analysis, it is characterized in that: described on-line analysis system (5) is by the automatic six-way valve of two series connection, the permanent gases analysis systems such as hydrogen, carbon monoxide, carbon dioxide, hydro carbons C
1-C
4hydrocarbon analysis system, oil phase product is C
5-C
7non-aromatics and aromatic hydrocarbons and methyl alcohol analytic system composition.
3. the online sampling of system and the method for analyzing described in claim 1 or 2, is characterized in that: comprise the steps:
Step 1: draw logistics: draw one aromizing product material from the outlet of reactor or middle device (1) by logistics ejector (2);
Step 2: system insulation: be incubated to the equipment and the pipeline that enter on-line analysis system (5) from logistics ejector (2), guarantee the not condensation in gas solid separation and filter process of aromizing product material;
Step 3: gas solid separation: remove entrained catalyzer in the aromizing product material that step 1 draws;
Step 4: filter: further remove the catalyst fines in aromizing product material after gas solid separation;
Step 5: on-line analysis: the aromizing product material after filtering is passed into on-line analysis system (5) and analyzes, analyze the composition of permanent gases wherein, methyl alcohol, water, aromatic hydrocarbon product.
4. the method for online sampling according to claim 3 and analysis, is characterized in that: the aromizing product material of drawing described in step 1 is aromatization of methanol or C
2-C
6the product of aromatization of hydrocarbons, it specifically consists of hydrogen, C
1-C
4hydro carbons and C
5-C
10non-aromatics and aromatic hydrocarbons, and water, methyl alcohol, carbon monoxide, carbon dioxide.
5. the method for online sampling according to claim 3 and analysis, is characterized in that: described in step 2, the temperature of system insulation is 180-300 ℃.
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|---|---|
| CN103913527B (en) | 2017-02-15 |
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