CN113957551B - Production method of industrial filament of high-strength high-modulus chinlon 66 - Google Patents
Production method of industrial filament of high-strength high-modulus chinlon 66 Download PDFInfo
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- CN113957551B CN113957551B CN202111376386.2A CN202111376386A CN113957551B CN 113957551 B CN113957551 B CN 113957551B CN 202111376386 A CN202111376386 A CN 202111376386A CN 113957551 B CN113957551 B CN 113957551B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
- D01D5/16—Stretch-spinning methods using rollers, or like mechanical devices, e.g. snubbing pins
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/08—Interlacing constituent filaments without breakage thereof, e.g. by use of turbulent air streams
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
- Yarns And Mechanical Finishing Of Yarns Or Ropes (AREA)
Abstract
The invention provides a production method of a high-strength high-modulus chinlon 66 industrial filament, which improves the crystallinity and the orientation degree of a chinlon 66 polymer by adjusting a drafting ratio, a drafting temperature, a setting temperature and a setting ratio, thereby achieving the purpose of improving the strength and the modulus of the chinlon 66 industrial filament. The industrial nylon-66 filament produced by the method has high strength, and the strength level can reach 9.9-10.5 g/d; the modulus is high, the 2% fixed elongation load of 1400dtex industrial yarn can reach 12.5N-15.3N, the 4% fixed elongation load can reach 19.7N-26.1N, the 8% fixed elongation load can reach 48.3N-70.7N, and the 12% fixed elongation load can reach 90.2N-125.9N, namely the nylon 66 industrial filament produced by the invention has high modulus, is not easy to deform, improves the dimensional stability of the tire, and prolongs the service life of the tire.
Description
Technical Field
The invention relates to the technical field of chemical fiber industrial filament production, in particular to a production method of a high-strength high-modulus nylon 66 industrial filament.
Background
The existing production methods of nylon 66 industrial filaments comprise two methods: one is continuous polymerization direct spinning; the other is chip melt spinning. The melt of the continuous polymerization direct spinning or the chip melt spinning needs to pass through a spinning assembly to form industrial nylon 66 filaments, and the spinning viscosity (formic acid relative viscosity) is between 69 and 80. The nylon 66 nascent fiber is extruded by a spinneret plate of a spinning assembly and then is subjected to drafting treatment by drafting equipment.
After being discharged from a spinneret plate, industrial nylon 66 filaments pass through a feeding roller, a 1 st pair of drafting rollers, a 2 nd pair of drafting rollers, a 3 rd pair of drafting rollers and a 4 th pair of drafting rollers and then enter a winding machine through a yarn guide to form a yarn tube. The industrial nylon 66 filament needs to be stretched twice before forming a filament tube, the first stretching is carried out between a first drafting roller and a second drafting roller, the second stretching is carried out between a second drafting roller and a third drafting roller, the first drafting ratio is 2.5-3.3, the total drafting ratio is 4.5-6.0, and the winding speed is 2300 m/min-3800 m/min.
The physical properties of the industrial nylon-66 filament produced by the process take 1400dtex as an example: the 2% constant elongation load is 9.7N-10.3N (namely the modulus is 3.898 GPa-4.14 GPa); the 4% constant elongation load is 15.4N-16.5N; 8% fixed elongation load 35.3N-37.5N; a 12% constant elongation load of 71.3N to 76.8N; the strength is about 9.6 g/d; the breaking elongation is between 16 and 22 percent; the constant load elongation is between 10.5 and 13.5 percent; the dry heat shrinkage is between 4.5 and 7.7 percent. The modulus of the nylon 66 industrial filament directly influences the modulus of the nylon 66 dipped cord, and the deformation of the tire in the use process is influenced after the dipped cord is manufactured into the tire. Therefore, in order to further improve the quality of the tire, the development of the high-strength and high-modulus nylon 66 is continuously pursued in the field.
Disclosure of Invention
In order to solve the technical problem that the industrial filament modulus of the chinlon 66 produced by the existing process is not high, the invention provides a production method of the industrial filament of the chinlon 66 with high strength and high modulus, and the crystallinity and the orientation degree of a chinlon 66 polymer are improved by adjusting the drawing temperature, the setting temperature and the setting ratio, so that the aim of improving the strength and the modulus of the industrial filament of the chinlon 66 is fulfilled.
The invention adopts the following technical scheme:
a production method of industrial filaments of high-strength high-modulus chinlon 66 comprises the following steps: (1) The molten nylon 66 polymer is spun by a spinneret plate to form nylon 66 nascent fiber;
(2) Cooling the nylon 66 nascent fiber formed in the step (1) by cooling air;
(3) Oiling the cooled chinlon 66 nascent fiber in the step (2) after passing through a spinning channel;
(4) Bundling the chinlon 66 nascent fiber subjected to the oiling treatment in the step (3), and performing pre-network treatment on the chinlon 66 nascent fiber;
(5) Feeding the nylon 66 nascent fiber obtained in the step (4) onto a multi-stage drafting device, wherein the multi-stage drafting device comprises at least 4 pairs of hot rollers, and the nylon 66 nascent fiber is sequentially wound on the hot rollers;
the hot roller comprises at least three pairs of drafting rollers and at least one pair of shaping rollers arranged after the drafting roller process, wherein the temperature of the last pair of drafting rollers is 205-245 ℃.
(6) After coming out of the multistage drafting equipment, the industrial nylon-66 filaments are subjected to network treatment by a network machine and then enter a winding machine to be wound into a filament tube.
Furthermore, the diameter of the spinneret plate is 0.23-0.45 mm, and the length-diameter ratio is 1.
Further, the multistage drafting equipment comprises 4 pairs of hot rollers, wherein the first three pairs of hot rollers are drafting rollers, the second pair of hot rollers are shaping rollers, the temperature of the first drafting roller is 50-65 ℃, the temperature of the second drafting roller is 190-210 ℃, the temperature of the third drafting roller is 205-245 ℃, and the temperature of the fourth shaping roller is 130-190 ℃; the setting ratio is 0.972-0.982.
Further, the multistage drafting equipment comprises 5 pairs of hot rollers, wherein the first three pairs of hot rollers are drafting rollers, the second two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller is 50-65 ℃, the temperature of the second drafting roller is 190-210 ℃, the temperature of the third drafting roller is 205-245 ℃, the temperature of the fourth shaping roller is 160-200 ℃, and the temperature of the fifth shaping roller is 120-160 ℃; the setting ratio was 1.002.
Further, the multistage drafting equipment comprises 6 pairs of hot rollers, wherein the front four pairs of hot rollers are drafting rollers, the back two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller is 40-50 ℃, the temperature of the second drafting roller is 50-65 ℃, the temperature of the third drafting roller is 200-220 ℃, the temperature of the fourth drafting roller is 220-245 ℃, the temperature of the fifth shaping roller is 180-200 ℃, and the temperature of the sixth shaping roller is 130-160 ℃; the setting ratio was 0.953.
Compared with the prior art, the invention has the following technical effects:
1. the industrial nylon-66 filament produced by the method has the characteristics of high strength and high modulus. The invention achieves the purpose of producing the high-strength high-modulus nylon 66 industrial yarn by properly increasing the drafting temperature, reducing the setting temperature and increasing the setting ratio.
2. The industrial nylon 66 filament produced by the method has high strength, the strength level can reach 9.9-10.5 g/d, the increase of the strength can reduce the use amount of the dipped cord fabric in the tire, and the weight of the tire is reduced.
3. The industrial nylon 66 filament produced by the method has high modulus, the 2% fixed elongation load of 1400dtex industrial filament can reach 12.5N-15.3N, the 4% fixed elongation load can reach 19.7N-26.1N, the 8% fixed elongation load can reach 48.3N-70.7N, and the 12% fixed elongation load can reach 90.2N-125.9N. The industrial nylon-66 filament has high modulus, less deformation, raised fatigue resistance and long service life.
Detailed Description
The present invention will be further described with reference to the following specific embodiments.
In order to express the modulus of the nylon 66 industrial yarn more simply and conveniently, the modulus level of the nylon 66 industrial yarn is measured by constant elongation loads of 2%, 4%, 8% and 12%.
A production method of industrial filaments of high-strength high-modulus chinlon 66 comprises the following steps:
(1) The molten nylon 66 polymer is spun by a spinneret plate to form nylon 66 nascent fiber; the diameter of the spinneret plate is 0.23-0.45 mm, and the length-diameter ratio is 1;
(2) Cooling the nylon 66 nascent fiber formed in the step (1) by cooling air;
(3) Oiling the cooled chinlon 66 nascent fiber in the step (2) after passing through a spinning channel;
(4) Bundling the chinlon 66 nascent fiber subjected to the oiling treatment in the step (3), and performing pre-network treatment on the chinlon 66 nascent fiber;
(5) Enabling the nylon 66 nascent fiber obtained in the step (4) to enter a multi-stage drafting device, wherein the multi-stage drafting device comprises at least 4 pairs of hot rollers, and sequentially winding the nylon 66 nascent fiber on the hot rollers until no available hot rollers exist;
the hot roller comprises at least three pairs of drafting rollers and at least one pair of shaping rollers arranged after the drafting roller process, wherein the temperature of the last pair of drafting rollers is 205-245 ℃. The shaping roller gradually relaxes the drawn chinlon 66 industrial filaments.
When the multistage drafting equipment comprises 4 pairs of hot rollers, the nylon 66 nascent fiber obtained in the step (4) is wound on a feeding roller, and then enters the multistage drafting equipment, and the feeding roller is not provided with a heating device. The front three pairs of hot rollers in the 4 pairs of hot rollers are drafting rollers, the back pair of hot rollers are shaping rollers, the temperature of the first drafting roller is 50-65 ℃, the temperature of the second drafting roller is 190-210 ℃, the temperature of the third drafting roller is 205-245 ℃, and the temperature of the fourth shaping roller is 130-190 ℃; the setting ratio is 0.972-0.982.
When the multistage drafting equipment comprises 5 pairs of hot rollers, the nylon 66 nascent fiber obtained in the step (4) is wound on a feeding roller, and then enters the multistage drafting equipment, and the feeding roller is not provided with a heating device. The front three pairs of hot rollers in the 5 pairs of hot rollers are drafting rollers, the back two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller is 50-65 ℃, the temperature of the second drafting roller is 190-210 ℃, the temperature of the third drafting roller is 205-245 ℃, the temperature of the fourth shaping roller is 160-200 ℃, and the temperature of the fifth shaping roller is 120-160 ℃; the setting ratio was 1.002.
When the multistage drafting equipment comprises 6 pairs of hot rollers, the front four pairs of hot rollers are drafting rollers, the rear two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller is 40-50 ℃, the temperature of the second drafting roller is 50-65 ℃, the temperature of the third drafting roller is 200-220 ℃, the temperature of the fourth drafting roller is 220-245 ℃, the temperature of the fifth shaping roller is 180-200 ℃, and the temperature of the sixth shaping roller is 130-160 ℃; the setting ratio was 0.953.
The invention achieves the purpose of producing the high-strength and high-modulus nylon 66 industrial yarn by properly increasing the drafting temperature (namely increasing the temperature of the drafting rollers, particularly the temperature of the last pair of drafting rollers), reducing the setting temperature (namely reducing the temperature of the setting rollers, particularly the temperature of the last pair of setting rollers) and increasing the setting ratio and the total drafting ratio.
(6) The industrial nylon-66 filament is taken out from the multistage drafting equipment, is subjected to network treatment by a network machine, and then enters a winding machine to be wound into a filament tube, wherein the winding speed is 2300-2885 m/min.
The shaping ratio is the ratio of the roller speed of the last pair of shaping rollers to the roller speed of the last pair of drafting rollers;
the total draft ratio is the ratio of the speed of the last pair of draft rollers to the speed of the first pair of draft rollers.
The invention realizes the high consistency of the polymer micro-molecular arrangement by adjusting the setting ratio and the total draft ratio, thereby realizing the purpose of improving the orientation degree and the crystallinity degree of the polymer, the draft temperature is improved in order to give enough energy to the polymer to enable the polymer to generate relative sliding of molecular chains, and the setting temperature is reduced in order to rapidly cool and fix the orientation degree and the crystallinity degree of the existing polymer by the drawn tows, and prevent the orientation degree and the crystallinity degree of the fiber from being reduced after the fiber is rapidly shrunk.
The application example adopting the method is as follows:
in examples 1 to 4, the produced nylon 66 industrial filament is 1400dtex industrial filament, the multistage drafting equipment adopted in the production process comprises 4 pairs of hot rollers, wherein the front three hot rollers in the 4 pairs of hot rollers are drafting rollers, the rear hot roller pair is a shaping roller, the temperature of the first drafting roller (1G for short) is 50 ℃ to 65 ℃, the temperature of the second drafting roller (2G for short) is 190 ℃ to 210 ℃, the temperature of the third drafting roller (3G for short) is 205 ℃ to 245 ℃, and the temperature of the fourth shaping roller (4G for short) is 130 ℃ to 190 ℃. The parameter settings for each example are shown in table 1.
In examples 5 to 6, the industrial nylon-66 filament was 940dtex, and the multi-stage drawing apparatus used in the production process included 4 pairs of hot rolls. The parameter settings for each example are shown in table 1.
In the comparative example, the industrial nylon 66 filament is 1400dtex, and the multistage drafting equipment adopted in the production process comprises 4 pairs of hot rollers. The parameter settings for each example are shown in table 1.
TABLE 1
As can be seen from Table 1, examples 1-6 have higher strength and modulus than the comparative examples; 1G and 2G temperature changes have little or no influence on the modulus; 3G and 4G temperature changes have large influence on the modulus; example 4 is a preferred example.
In examples 7 to 10, the produced nylon-66 industrial filament was 1400dtex industrial filament, and the multi-stage drawing apparatus used in the production process included 5 pairs of hot rolls. The multistage drafting equipment comprises 5 pairs of hot rollers, wherein the first three pairs of hot rollers are drafting rollers, the second two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller (1G for short) is 50-65 ℃, the temperature of the second drafting roller (2G for short) is 190-210 ℃, the temperature of the third drafting roller (3G for short) is 205-245 ℃, the temperature of the fourth shaping roller (4G for short) is 160-200 ℃, and the temperature of the fifth shaping roller (5G for short) is 120-160 ℃. The parameter settings for each example are shown in table 2.
TABLE 2
As can be seen from Table 2, the 5G set temperature and the 3G draft temperature have a large influence on the modulus, and example 7 is a preferred example.
In examples 11 to 13, the industrial nylon 66 filaments were 467dtex industrial filaments, and the multistage drafting equipment used in the production process included 6 pairs of hot rolls. The multistage drafting equipment comprises 6 pairs of hot rollers, wherein the front four pairs of hot rollers are drafting rollers, the rear two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller (1G for short) is 40-50 ℃, the temperature of the second drafting roller (2G for short) is 50-65 ℃, the temperature of the third drafting roller (3G for short) is 200-220 ℃, the temperature of the fourth drafting roller (4G for short) is 220-245 ℃, the temperature of the fifth shaping roller (5G for short) is 180-200 ℃, and the temperature of the sixth shaping roller (6G for short) is 130-160 ℃. The parameter settings for each example are shown in table 3.
TABLE 3
As can be seen from Table 3, examples 11-13 all use 6 pairs of hot rolls, which are the evidences of process adjustment of examples 1-10 on the one hand, and on the other hand, it can be seen that the more drawing rolls of the equipment, the more beneficial the development of high strength and high modulus products. Example 11 is a preferred example.
Examples of the method of converting the constant elongation load include: when the 2% constant elongation load of 940dtex was 9.3N, the data of 1400dtex constant elongation load was 9.3 × 1400/940=13.85N, and when the data of 467dtex constant elongation load was 5.1N, the data of 1400dtex constant elongation load was 5.1 × 1400/467=15.3N.
The above-mentioned embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, and it is obvious to those skilled in the art that other embodiments can be easily made by replacing or changing the technical contents disclosed in the present specification, and therefore, the changes and modifications made by the principles and process conditions of the present invention should be included in the claims of the present invention.
Claims (2)
1. A production method of industrial filaments of high-strength high-modulus chinlon 66 is characterized by comprising the following steps:
(1) The melted nylon 66 polymer is spun out by a spinneret plate to form nylon 66 nascent fiber;
(2) Cooling the nylon 66 nascent fiber formed in the step (1) by cooling air;
(3) Oiling the cooled chinlon 66 nascent fiber in the step (2) after passing through a spinning channel;
(4) Bundling the chinlon 66 nascent fiber subjected to the oiling treatment in the step (3), and performing pre-network treatment on the chinlon 66 nascent fiber;
(5) Enabling the nylon 66 nascent fiber obtained in the step (4) to enter a multi-stage drafting device, wherein the multi-stage drafting device comprises at least 4 pairs of hot rollers, and the nylon 66 nascent fiber is sequentially wound on the hot rollers;
the at least 4 pairs of hot rollers comprise at least three pairs of drafting rollers and at least one pair of shaping rollers arranged after the drafting roller process, and the temperature of the last pair of drafting rollers is 205-245 ℃;
when the multistage drafting equipment comprises 4 pairs of hot rollers, the front three pairs of hot rollers are drafting rollers, the rear pair of hot rollers are setting rollers, the temperature of the first drafting roller is 50-65 ℃, the temperature of the second drafting roller is 190-210 ℃, the temperature of the third drafting roller is 205-245 ℃, and the temperature of the fourth setting roller is 130-190 ℃; the setting ratio is 0.972-0.982; the total draft ratio is 5.300-5.329;
when the multistage drafting equipment comprises 5 pairs of hot rollers, the front three pairs of hot rollers are drafting rollers, the rear two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller is 50-65 ℃, the temperature of the second drafting roller is 190-210 ℃, the temperature of the third drafting roller is 205-245 ℃, the temperature of the fourth shaping roller is 160-200 ℃, and the temperature of the fifth shaping roller is 120-160 ℃; setting ratio is 1.002; the total draft ratio is 5.4;
the multistage drafting equipment comprises 6 pairs of hot rollers, wherein the front four pairs of hot rollers are drafting rollers, the rear two pairs of hot rollers are shaping rollers, the temperature of the first drafting roller is 40-50 ℃, the temperature of the second drafting roller is 50-65 ℃, the temperature of the third drafting roller is 200-220 ℃, the temperature of the fourth drafting roller is 220-245 ℃, the temperature of the fifth shaping roller is 180-200 ℃, and the temperature of the sixth shaping roller is 130-160 ℃; the setting ratio is 0.953; the total draw ratio was 5.224;
(6) After coming out of the multistage drafting equipment, the industrial nylon-66 filaments are subjected to network treatment by a network machine and then enter a winding machine to be wound into a filament tube.
2. The method for producing the industrial filament of the high-strength high-modulus nylon 66 as claimed in claim 1, wherein the diameter of the spinneret plate is 0.23-0.45 mm, and the length-diameter ratio is 1.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111376386.2A CN113957551B (en) | 2021-11-19 | 2021-11-19 | Production method of industrial filament of high-strength high-modulus chinlon 66 |
| PCT/CN2022/094663 WO2023087650A1 (en) | 2021-11-19 | 2022-05-24 | Production method for high-strength and high-modulus nylon 66 industrial filament |
| ZA2022/08252A ZA202208252B (en) | 2021-11-19 | 2022-07-25 | Production method of high-strength and high-modulus industrial polyamide (pa) 66 filament yarn |
| LU502580A LU502580B1 (en) | 2021-11-19 | 2022-07-27 | Production method of high-strength and high-modulus industrial polyamide (pa) 66 filament yarn |
Applications Claiming Priority (1)
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| CN202111376386.2A CN113957551B (en) | 2021-11-19 | 2021-11-19 | Production method of industrial filament of high-strength high-modulus chinlon 66 |
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| CN113957551A CN113957551A (en) | 2022-01-21 |
| CN113957551B true CN113957551B (en) | 2022-12-02 |
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| CN (1) | CN113957551B (en) |
| LU (1) | LU502580B1 (en) |
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| CN113957551B (en) * | 2021-11-19 | 2022-12-02 | 平顶山神马帘子布发展有限公司 | Production method of industrial filament of high-strength high-modulus chinlon 66 |
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| WO2023087650A1 (en) | 2023-05-25 |
| ZA202208252B (en) | 2022-10-26 |
| CN113957551A (en) | 2022-01-21 |
| LU502580B1 (en) | 2023-01-30 |
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