LU501352B1 - Method for Preparing Metal-Organic Framework Material by Using Metallurgical Mine Solid Waste - Google Patents
Method for Preparing Metal-Organic Framework Material by Using Metallurgical Mine Solid Waste Download PDFInfo
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- LU501352B1 LU501352B1 LU501352A LU501352A LU501352B1 LU 501352 B1 LU501352 B1 LU 501352B1 LU 501352 A LU501352 A LU 501352A LU 501352 A LU501352 A LU 501352A LU 501352 B1 LU501352 B1 LU 501352B1
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- solid waste
- organic
- mixed
- temperature
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- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 26
- 239000002910 solid waste Substances 0.000 title claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 28
- 238000000926 separation method Methods 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 150000003839 salts Chemical class 0.000 claims abstract description 19
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 239000013110 organic ligand Substances 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 8
- 239000002699 waste material Substances 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims description 26
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052742 iron Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 5
- SUAKHGWARZSWIH-UHFFFAOYSA-N N,N‐diethylformamide Chemical compound CCN(CC)C=O SUAKHGWARZSWIH-UHFFFAOYSA-N 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000428 dust Substances 0.000 abstract description 13
- 229910001092 metal group alloy Inorganic materials 0.000 abstract description 6
- 239000002893 slag Substances 0.000 abstract description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 5
- 239000011707 mineral Substances 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 229910000831 Steel Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000012300 argon atmosphere Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F15/00—Compounds containing elements of Groups 8, 9, 10 or 18 of the Periodic Table
- C07F15/02—Iron compounds
- C07F15/025—Iron compounds without a metal-carbon linkage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention belongs to the field of comprehensive utilization of resources, in particular to a method for preparing a metal-organic framework (MOF) material by using metallurgical mine solid waste. The method uses concentrated strong acid or strong alkali to dissolve the metallurgical mine solid waste to obtain mixed metal salt. An organic matter is used as an organic ligand. The mixed metal salt and the organic ligand are dissolved in an organic solvent. The mixture is kept at a constant temperature of 70-150°C for 18-30 h, thus synthesizing an MOF material. The present invention provides a new method for preparing the MOF material containing valuable metal elements by using the metallurgical mine solid waste. Raw materials are readily available; metallurgical slag containing valuable metal elements, minerals, dust, and other waste metal alloys can be effectively exploited. The synthesis method is simple, and synthesis conditions are mild. The method is applicable to comprehensive utilization of the metallurgical slag, the minerals, the dust, and the waste metal alloys. Drawing of the Abstract Mix a metallurgical mine solid waste with concentrated strong acid or strong alkali to obtain mixed metal salt Dissolve the mixed metal salt in an organic solvent to obtain a first solution Dissolve an organic ligand in the organic solvent to obtain a second solution Uniformly mix the first solution with the second solution to obtain a mixed solution, put the mixed solution into a hydrothermal reaction kettle, and dry to obtain a solid- liquid mixture Heat the solid-liquid mixture obtained for constant- temperature separation to obtain solid powder Dry, at a constant temperature, the obtained solid powder under an oxygen-free environment to obtain a metal- organic framework material
Description
Description Method for Preparing Metal-Organic Framework Material by Using Metallurgical Mine Solid Waste
TECHNICAL FIELD The present invention belongs to the field of comprehensive utilization of resources, and relates to a method for preparing a metal-organic framework (MOF) material by using metallurgical mine solid waste.
BACKGROUND There are a large amount of metal element-containing metallurgical slag, minerals, dust, and a large number of iron-containing waste metal alloys in China. The annual output of blast furnace slag is as high as 200 million tons or more. There are more than 400 tailings ponds in all sizes. More than 5 billion tons of tailings are stacked in all metal mines, and the annual growth rate of the tailings is 0.5 billion tons. In recent years, there are nearly 0.28 million tons of stainless steel dust output every year in China. Dust contains Fe, Cr, Ti, and other valuable metals. Meanwhile, a series of iron-containing metal alloy such as a large amount of scrap steel are output, and the comprehensive utilization value is extremely high. Traditional valuable metal recycling has problems of high energy consumption and high pollution. Providing a new method is of great significance. A metal-organic framework (MOF) material is mainly a three-dimensional network structure crystal material formed by hybridizing of nitrogen and oxygen multidentate organic ligands of aromatic acid or alkali by an inorganic metal center. At the same time, the MOF material has a large specific surface area, a large porosity, and a 1 functional pore and channel structure, which can effectively store energy gas. Due to its structural characteristics, the MOF material has excellent performance in gas-liquid phase separation, and also has good catalysis, optical, magnetic properties, etc. The preparation method is provided not only to achieve recycling of resource solid wastes, but also provides a new idea for the preparation of the MOF materials, which can prepare high value-added materials and has high application value.
SUMMARY An embodiment of the present disclosure discloses a method for preparing a metal-organic framework (MOF) material by using metallurgical mine solid waste, so as to solve any one of the above-mentioned and other potential problems in the prior art.
In order to achieve the above object, the embodiment of the present disclosure discloses a method for preparing an MOF material by using metallurgical mine solid waste. The method specifically includes the following steps: S1) mixing a metallurgical mine solid waste with concentrated strong acid or strong alkali to fully dissolve the metallurgical mine solid waste, then performing centrifuging, filtering, and separation, and performing drying in a drying oven at a constant temperature to obtain mixed metal salt; S2) dissolving the mixed metal salt in an organic solvent to obtain a first solution; S3) dissolving an organic ligand in the organic solvent to obtain a second solution; S4) uniformly mixing the first solution obtained at S2) with the second solution 2 obtained at S3) to obtain a mixed solution, putting the mixed solution into a hydrothermal reaction kettle, keeping the mixed solution in the drying oven at a constant temperature for certain time to obtain a solid-liquid mixture; SS) heating the solid-liquid mixture obtained at S4) for constant-temperature separation to obtain solid powder; and S6) drying, at a constant temperature, the solid powder obtained at S5) under an oxygen-free environment.
According to the embodiment of the present disclosure, the specific process of S1) is as follows: a ratio of the volume of an iron-containing waste to the volume of the concentrated strong acid or strong alkali is 3-5: 4-6; a centrifugal separation factor Fr is controlled at 7000-10000; the drying temperature is 70-150°C; and the drying time is 12-36 h.
According to the embodiment of the present disclosure, the metallurgical mine solid waste at S1) has a particle size of 50-250 microns; the concentrated strong acid is concentrated sulfuric acid, concentrated hydrochloric acid, or concentrated nitric acid, and the strong alkali is sodium hydroxide or potassium hydroxide.
According to the embodiment of the present disclosure, the process at S2) is as follows: a feeding ratio of the mixed metal salt is 13-133 mg/ml, and ultrasonic treatment is performed for 2-5 min.
According to the embodiment of the present disclosure, the process at S3) is as follows: a feeding ratio of the organic ligand is 5-50 mg/ml, and ultrasonic treatment
3 is performed for 2-5 min.
According to the embodiment of the present disclosure, the organic solvent in S2) and S3) is dimethylformamide, dimethylacetamide, diethylformamide, or ethanol.
According to the embodiment of the present disclosure, the organic ligand in S3) is CsHsO4, C14H1004, CAH6N2, or CoHgOg.
According to the embodiment of the present disclosure, the process in S5) is as follows: the temperature is 70-150°C, and the constant-temperature treatment time is 18-30 h.
According to the embodiment of the present disclosure, the process in S6) is as follows: the drying temperature is 40-90°C, and the drying time is 8-20 h.
An MOF framework material is prepared by the above method.
The present invention has the following characteristics: (1) In the present invention, a method for exploiting metallurgical slag of a steel plant, minerals, dust, and waste metal alloy is provided. (2) In this method, synthesis is realized at a relatively low temperature without the requirements of high temperature, high oxygen, and external high pressure. (3) Compared with traditional utilization of solid waste, the method effectively reduces the energy consumption and has a great guidance significance for providing a brand-new idea for the recycling of the metallurgical slag of the steel plant, minerals,
4 dust, and waste metal alloys.
BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flowchart of a method for preparing a metal-organic framework (MOF) material by using metallurgical mine solid waste.
DETAILED DESCRIPTION The specific examples described here are only used for explaining the present invention, and are not intended to limit the present invention. Those skilled in the art should understand that the method of the present invention is not only limited to preparing a metal-organic framework (MOF) material containing valuable metal elements by using metallurgical mine solid waste. The specific examples of the present invention are now described below. As shown in Fig. 1, an embodiment of the present disclosure discloses a method for preparing an MOF material by using metallurgical mine solid waste. The method specifically includes the following steps: S1) a metallurgical mine solid waste is mixed with concentrated strong acid or strong alkali to fully dissolve the metallurgical mine solid waste; centrifuging, filtering, and separation are then performed; drying is performed in a drying oven at a constant temperature to obtain mixed metal salt; S2) the mixed metal salt is dissolved in an organic solvent to obtain a first solution; S3) an organic ligand is dissolved in the organic solvent to obtain a second solution;
S4) the first solution obtained at S2) is uniformly mixed with the second solution obtained at S3) to obtain a mixed solution; the mixed solution is put into a hydrothermal reaction kettle and kept at a constant temperature in the drying oven for certain time, and a solid-liquid mixture is obtained, SS) the solid-liquid mixture obtained at S4) is heated for constant-temperature separation to obtain solid powder; and S6) the solid powder obtained at S5) is dried at a constant temperature under an oxygen-free environment.
According to the embodiment of the present disclosure, the specific process of S1) is as follows: a ratio of the volume of an iron-containing waste to the volume of the concentrated strong acid or strong alkali is 3-5: 4-6; a centrifugal separation factor Fr is controlled at 7000-10000; the drying temperature is 70-150°C; and the drying time is 12-36 h.
According to the embodiment of the present disclosure, the metallurgical mine solid waste at S1) has a particle size of 50-250 microns; the concentrated strong acid is concentrated sulfuric acid, concentrated hydrochloric acid, or concentrated nitric acid, and the strong alkali is sodium hydroxide or potassium hydroxide.
According to the embodiment of the present disclosure, the process at S2) is as follows: a feeding ratio of the mixed metal salt is 13-133 mg/ml, and ultrasonic treatment is performed for 2-5 min.
According to the embodiment of the present disclosure, the process at S3) is as
6 follows: a feeding ratio of the organic ligand is 5-50 mg/ml, and ultrasonic treatment is performed for 2-5 min.
According to the embodiment of the present disclosure, the organic solvent in S2) and S3) is dimethylformamide, dimethylacetamide, diethylformamide, or ethanol. According to the embodiment of the present disclosure, the organic ligand in S3) is CsHsO4, C14H1004, CAH6N2, or CoHgOg. According to the embodiment of the present disclosure, the process in S5) is as follows: the temperature is 70-150°C, and the constant-temperature treatment time is 18-30 h. According to the embodiment of the present disclosure, the process in S6) is as follows: the drying temperature is 40-90°C, and the drying time is 8-20 h. An MOF framework material is prepared by the above method. Example 1 S1) 80 g of dust (particle size of which was 200 microns) of a certain steel plant in China was mixed with 100 mL of concentrated strong acid; after the dust was dissolved, centrifuging, filtering, and separation were performed (a centrifugal separation factor Fr was controlled at 7000); and the obtained liquid was kept at a constant temperature of 120°C in a drying oven for 24 h to obtain mixed salt. S2) 1.2 g of the mixed salt was added to 15 ml of dimethylacetamide, and ultrasonic treatment was performed for 5 min to obtain a first solution.
7
S3) 0.2 g of CsHsOs4 was added to 15 ml of dimethylacetamide, and ultrasonic treatment was performed for 5 min to obtain a second solution. S4) The first solution and the second solution were mixed, and ultrasonic treatment was performed for 3 min to obtain a mixed solution. S5) The mixed solution was transferred into a 40mL stainless steel hydrothermal reaction kettle and kept at a constant temperature of 110°C for 20 h; after the reaction was completed, a solid-liquid mixture obtained by the reaction was subjected to suction filtration and separation, and was washed with alcohol for 4 times. S6) The powder obtained by separation was dried in an argon atmosphere at 60°C for 12 h to obtain an MOF material. Example 2 S1) 80 g of dust (particle size of which was 200 microns) of a certain steel plant in China was mixed with 100 mL of concentrated strong acid; after the dust was dissolved, centrifuging, filtering, and separation were performed (a centrifugal separation factor Fr was controlled at 8500); and the obtained liquid was kept at a constant temperature of 120°C in a drying oven for 24 h to obtain mixed salt. S2) 0.6 g of the mixed salt was added to 15 ml of dimethylformamide, and ultrasonic treatment was performed for 3 min to obtain a first solution. S3) 0.1 g of CsHsN, was added to 15 ml of dimethylformamide, and ultrasonic treatment was performed for 3 min to obtain a second solution.
8
S4) The first solution and the second solution were mixed, and ultrasonic treatment was performed for 3 min to obtain a mixed solution. S5) The mixed solution was transferred into a 40mL stainless steel hydrothermal reaction kettle and kept at a constant temperature of 110°C for 20 h; after the reaction was completed, a solid-liquid mixture obtained by the reaction was subjected to suction filtration and separation, and was washed with alcohol for 4 times. S6) The powder obtained by separation was dried in an argon atmosphere at 60°C for 12 h to obtain an MOF material. Example 3 S1) 80 g of dust (particle size of which was 200 microns) of a certain steel plant in China was mixed with 100 mL of concentrated strong acid; after the dust was dissolved, centrifuging, filtering, and separation were performed (a centrifugal separation factor Fr was controlled at 10000); and the obtained liquid was kept at a constant temperature of 120°C in a drying oven for 24 h to obtain mixed salt. S2) 0.2 g of the mixed salt was added to 15 ml of diethylformamide, and ultrasonic treatment was performed for 3 min to obtain a first solution. S3) 0.4 g of CsH6O4 was added to 45 ml of diethylformamide, and ultrasonic treatment was performed for 3 min to obtain a second solution. S4) The first solution and the second solution were mixed, and ultrasonic treatment was performed for 3 min to obtain a mixed solution.
9
S5) The mixed solution was transferred into a 70mL stainless steel hydrothermal reaction kettle and kept at a constant temperature of 110°C for 20 h; after the reaction was completed, a solid-liquid mixture obtained by the reaction was subjected to suction filtration and separation, and was washed with alcohol for 4 times.
S6) The powder obtained by separation was dried in an argon atmosphere at 60°C for 12 h to obtain an MOF material.
The above descriptions are only the preferred embodiments of the present invention, and are not intended to limit the scope of patent protection of the present invention.
Any equivalent structure transformation made by using the content of the specification and drawings of the present invention and directly or indirectly applied to other related technical fields shall all be similarly included in the scope of protection of the present invention.
Claims (10)
1. A method for preparing a metal-organic framework (MOF) material by using metallurgical mine solid waste, characterized by comprising the following steps: S1) mixing a metallurgical mine solid waste with concentrated strong acid or strong alkali to fully dissolve the metallurgical mine solid waste, then performing centrifuging, filtering, and separation, and performing drying in a drying oven at a constant temperature to obtain mixed metal salt; S2) dissolving the mixed metal salt in an organic solvent to obtain a first solution; S3) dissolving an organic ligand in the organic solvent to obtain a second solution; S4) uniformly mixing the first solution obtained at step S2 with the second solution obtained at step S3 to obtain a mixed solution, putting the mixed solution into a hydrothermal reaction kettle, keeping the mixed solution in the drying oven at a constant temperature for certain time to obtain a solid-liquid mixture; S5) heating the solid-liquid mixture obtained at step S4 for constant-temperature separation to obtain solid powder; and S6) drying, at a constant temperature, the solid powder obtained at step S5 under an oxygen-free environment.
2. The method according to claim 1, characterized in that the specific process of step S1 is as follows: a ratio of the volume of an iron-containing waste to the volume of the concentrated strong acid or strong alkali is 3-5: 4-6; a centrifugal separation factor Fr is controlled at 7000-10000; the drying temperature is 70-150°C; and the drying time is 12-36 h.
1
3. The method according to claim 1, characterized in that the metallurgical mine solid waste at step S1 has a particle size of 50-250 microns; the concentrated strong acid is concentrated sulfuric acid, concentrated hydrochloric acid, or concentrated nitric acid, and the strong alkali is sodium hydroxide or potassium hydroxide.
4. The method according to claim 1, characterized in that the process at step S2 is as follows: a feeding ratio of the mixed metal salt is 13-133 mg/ml, and ultrasonic treatment is performed for 2-5 min.
5. The method according to claim 1, characterized in that the process at step S3 is as follows: a feeding ratio of the organic ligand is 5-50 mg/ml, and ultrasonic treatment is performed for 2-5 min.
6. The method according to claim 1, characterized in that the organic solvent in step S2 and S3) is dimethylformamide, dimethylacetamide, diethylformamide, or ethanol.
7. The method according to claim 1, characterized in that the organic ligand in step S3 is CeH6O4, C14H1004, C4H6N3, or CoH606.
8. The method according to claim 1, characterized in that the process in step SS is as follows: the separation temperature is 70-150°C, and the constant-temperature treatment time 1s 18-30 h.
9. The method according to claim 1, characterized in that the process in step S6 1s as follows: the drying temperature is 40-90°C, and the drying time at a constant temperature 1s 8-20 h.
2
10. A metal-organic framework (MOF) material, characterized in that the MOF material is prepared by the method according to any one of claims 1 to 9. 3
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU501352A LU501352B1 (en) | 2022-01-28 | 2022-01-28 | Method for Preparing Metal-Organic Framework Material by Using Metallurgical Mine Solid Waste |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LU501352A LU501352B1 (en) | 2022-01-28 | 2022-01-28 | Method for Preparing Metal-Organic Framework Material by Using Metallurgical Mine Solid Waste |
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| LU501352B1 true LU501352B1 (en) | 2022-08-10 |
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