CN111593433A - Energy-storage heating fiber and preparation method thereof - Google Patents
Energy-storage heating fiber and preparation method thereof Download PDFInfo
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- CN111593433A CN111593433A CN202010458494.3A CN202010458494A CN111593433A CN 111593433 A CN111593433 A CN 111593433A CN 202010458494 A CN202010458494 A CN 202010458494A CN 111593433 A CN111593433 A CN 111593433A
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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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
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- D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
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Abstract
The invention discloses a preparation method of energy storage heating fiber and the energy storage heating fiber, which comprises preparing a first solution by using a tungsten source and a first surfactant, and preparing a second solution by using a cesium source and a second surfactant; mixing the first solution and the second solution to prepare a precursor sol; drying and annealing the precursor sol in sequence to prepare heat storage and heating filler nano powder; mixing the heat storage and heating filler nano powder with a polyester polymer, and granulating to obtain functional master batches; the method comprises the steps of preparing heat storage and heating filler nano powder by using a tungsten source and a cesium source, and further realizing the functions of effectively shielding infrared heat radiation and absorbing ultraviolet rays and having strong absorption in a near infrared region and an ultraviolet region of the energy storage and heating fiber by using the heat storage and heating filler nano powder.
Description
Technical Field
The invention relates to the technical field of chemical composite fibers, in particular to a preparation method of energy-storage heating fibers and the energy-storage heating fibers.
Background
The heating fiber is a novel fiber which can generate heat and keep warm. Along with the improvement of aesthetic and comfortable requirement of people, can generate heat and durable heat retaining frivolous surface fabric receives favour day by day, thereby the fibrous research and development of generating heat has been promoted, however present fibrous material that generates heat leads to the performance of generating heat inconsistent because the function that adopts adds the material difference, for example can only absorb light and generate heat, do not possess the heat retaining effect after generating heat, do not possess simultaneously can shield solar ultraviolet radiation, human thermal radiation and absorption infrared thermal radiation's function, and then lead to the performance of generating heat great difference or can not make full use of human self thermal radiation under the environment of difference and keep warm, thereby the travelling comfort that people wear the clothing that this type of material made has been reduced.
Disclosure of Invention
The invention provides a preparation method of energy storage heating fiber and the energy storage heating fiber, aiming at providing the energy storage heating fiber which can effectively shield solar ultraviolet radiation, human body thermal radiation and absorb infrared thermal radiation and has strong absorption function in near infrared region and ultraviolet region.
In order to achieve the aim, the invention provides a preparation method of an energy storage heating fiber, which comprises the following steps:
preparing a first solution by using a tungsten source and a first surfactant, and preparing a second solution by using a cesium source and a second surfactant;
mixing the first solution and the second solution to prepare a precursor sol;
drying and annealing the precursor sol in sequence to prepare heat storage and heating filler nano powder;
mixing the heat storage and heating filler nano powder with a polyester polymer, and granulating to obtain functional master batches;
and carrying out melt spinning on the functional master batch to prepare the energy storage heating fiber.
Preferably, adding a tungsten source and a first surfactant into a first solvent, stirring and mixing to obtain a first solution;
the cesium source and the second surfactant are added to the second solvent and mixed with stirring to obtain a second solution.
Preferably, the molar ratio of tungsten element in the tungsten source and cesium element in the cesium source is greater than or equal to 2, the tungsten source comprises one or more of tungsten chloride, tungstic acid, tungsten carbonyl, sodium tungstate, ammonium tungstate and tungsten ethoxide, and the cesium source comprises one or more of cesium chloride, cesium formate, cesium hydroxide, cesium carbonate, cesium nitrate, cesium sulfate, cesium acetate, cesium bicarbonate and cesium amide.
Preferably, the first surfactant and the second surfactant comprise one or more of lignosulfonate, heavy alkylbenzene sulfonate, alkyl sulfonate, cetyl trimethyl ammonium bromide, sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, citric acid, oxalic acid, L-cysteine, disodium ethylenediamine tetraacetate, lauroyl glutamic acid, sodium stearyl sulfate and sodium fatty alcohol polyoxyethylene ether sulfate, wherein the first surfactant and the second surfactant are different.
Preferably, the first solvent and the second solvent comprise one or more of deionized water, cyclohexane, ethanol and acetone.
Preferably, the second solution is dropped into the first solution at a predetermined speed, and the temperature of the first solution is controlled within a predetermined temperature range to prepare a precursor sol.
Preferably, the precursor sol is dried to produce a precursor xerogel;
calcining the precursor xerogel at the temperature of between 300 and 1200 ℃ for 0.5 to 12 hours, and naturally cooling to room temperature to prepare the heat storage and heating filler nano powder.
Preferably, the polyester polymer comprises one or more of polyamide, methylcellulose, polyacrylonitrile, viscose cellulose, polymethyl methacrylate, polyester, cellulose acetate, polyolefin, polyvinyl alcohol, cuprammonium cellulose, polyurethane, and polycarbonate.
Preferably, the method is characterized in that one or more of an open mill, an internal mixer, a single-screw extrusion granulator and a double-screw extrusion granulator are adopted to blend the heat storage and heat generation filler nano powder and the polyester polymer for in-out granulation.
In addition, in order to achieve the above purpose, an embodiment of the present invention further provides an energy storage heating fiber, and the energy storage heating fiber is prepared by the above preparation method of the energy storage heating fiber.
Compared with the prior art, the invention provides a preparation method of energy-storage heating fiber and the energy-storage heating fiber, wherein a first solution is prepared by utilizing a tungsten source and a first surfactant, a second solution is prepared by utilizing a cesium source and a second surfactant, the first solution and the second solution are mixed to prepare a precursor sol, then the precursor sol is sequentially dried and annealed to prepare heat-storage heating filler nano-powder, the heat-storage heating filler nano-powder and a polyester polymer are blended, fed and discharged for granulation to prepare a functional master batch, and the functional master batch is subjected to melt spinning to prepare the energy-storage heating fiber It has the functions of absorbing ultraviolet ray and absorbing light in near infrared region and ultraviolet region.
Drawings
FIG. 1 is a schematic flow chart of a first embodiment of the energy storage and heat generation fiber preparation method of the invention;
FIG. 2 is an X-ray diffraction diagram of a second embodiment of the energy storage and heat emitting fiber preparation method of the invention;
FIG. 3 is an electron microscope image of a second embodiment of the energy storage heating fiber preparation method of the present invention;
fig. 4 is an infrared thermal imaging diagram of a second embodiment of the energy storage heating fiber preparation method of the invention.
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a preparation method of energy storage heating fibers, and referring to fig. 1, fig. 1 is a schematic flow diagram of a first embodiment of the preparation method of the energy storage heating fibers, specifically, the method comprises the following steps:
step S10, preparing a first solution by using a tungsten source and a first surfactant, and preparing a second solution by using a cesium source and a second surfactant;
in the step, it can be understood that the heating fiber is a novel fiber capable of generating heat by itself and keeping warm, however, the heating performance of the existing heating fiber material is inconsistent due to different functional additives, so in order to prepare an energy storage heating fiber capable of effectively shielding solar ultraviolet radiation, human body thermal radiation and absorbing infrared thermal radiation and having strong absorption function in a near infrared region and an ultraviolet region, it is necessary to prepare a nano powder capable of effectively shielding solar ultraviolet radiation, human body thermal radiation and absorbing infrared thermal radiation and having strong absorption function in the near infrared region and the ultraviolet region.
In this embodiment, a tungsten source and a cesium source with excellent optical properties are used as raw materials to prepare a heat-storage and heat-generation filler nanopowder with excellent optical properties, specifically, a first solution is prepared by using the tungsten source and a first surfactant, and a second solution is prepared by using the cesium source and a second surfactant, wherein a molar ratio of tungsten element in the tungsten source to cesium element in the cesium source is greater than or equal to 2, the tungsten source includes one or more of tungsten chloride, tungstic acid, tungsten carbonyl, sodium tungstate, ammonium tungstate and tungsten ethoxide, and the cesium source includes one or more of cesium chloride, cesium formate, cesium hydroxide, cesium carbonate, cesium nitrate, cesium sulfate, cesium acetate, cesium bicarbonate and cesium amide.
Specifically, step S10 includes the steps of,
step S101, adding a tungsten source and a first surfactant into a first solvent, stirring and mixing to obtain a first solution;
step S102, a cesium source and a second surfactant are added to a second solvent and mixed with stirring to obtain a second solution.
In this step, a tungsten source and a first surfactant are respectively added to a first solvent and stirred to obtain a first solution, and a cesium source and a second surfactant are added to a second solvent and stirred to obtain a second solution, wherein in this embodiment, the first surfactant and the second surfactant include one or more of lignosulfonate, heavy alkylbenzene sulfonate, alkylsulfonate, cetyltrimethylammonium bromide, sodium dodecylbenzenesulfonate, polyvinylpyrrolidone, polyvinyl alcohol, citric acid, oxalic acid, L-cysteine, disodium ethylenediaminetetraacetate, lauroyl glutamic acid, sodium stearyl sulfate, and sodium fatty alcohol polyoxyethylene ether sulfate, wherein the first surfactant and the second surfactant are different, and the first solvent and the second solvent include deionized water, cyclohexane, deionized water, cyclohexane, sodium stearyl alcohol, and sodium polyoxyethylene ether sulfate, One or more of ethanol and acetone.
Further, based on the above tungsten source, first surfactant, cesium source, second surfactant, first solvent, and second solvent, an example of preparing the first solution and the second solution is provided, in which the tungsten source is tungsten hexachloride, the first surfactant is citric acid, the cesium source is cesium formate, and the second surfactant is sodium dodecylbenzenesulfonate, wherein the first solvent is a mixed solvent of deionized water and ethanol, and the second solvent is deionized water, specifically, 25g of tungsten hexachloride and 7.5g of citric acid are respectively weighed, and 25g of tungsten hexachloride and 7.5g of citric acid are mixed into a mixed solvent of 35mL of ethanol and 25mL of deionized water to prepare the first solvent, and 3.7g of cesium formate and 4g of sodium dodecylbenzenesulfonate are respectively weighed and added into 25mL of deionized water to prepare the second solvent.
Step S20, mixing the first solution and the second solution to prepare precursor sol;
in this step, after the first solution and the second solution are prepared, the first solution and the second solution are mixed to allow a reaction between the tungsten source under the action of the first surfactant and the cesium source under the action of the second surfactant to prepare a precursor sol.
In particular, this step comprises, in a first step,
step S201, dropping the second solution into the first solution at a predetermined speed, and controlling the temperature of the first solution within a predetermined temperature range to obtain a precursor sol.
In this step, for example, the second solution is dropped into the first solution at a rate of 1 drop/second, and the temperature of the first solution is controlled to be within a preset temperature range at any moment during the dropping process, it can be understood that, during the dropping process of the second solution into the first solution, since the substance in the second solution reacts with the substance in the first solution to generate heat or heat, the temperature of the first solution should be controlled to be within a preset temperature range during the dropping process, wherein the preset temperature range is an ambient temperature at which the substance in the first solution reacts with the substance in the second solution optimally.
Step S30, drying and annealing the precursor sol in sequence to prepare heat storage and heating filler nano powder;
after the precursor sol is prepared, drying the precursor sol at a high temperature, for example, placing the precursor sol in a drying oven for drying, and annealing after drying to prepare the heat storage and heating filler nano-powder.
In particular, this step comprises, in a first step,
step S301, drying the precursor sol to prepare a precursor xerogel;
and S302, calcining the precursor xerogel at 300-1200 ℃ for 0.5-12 h, and naturally cooling to room temperature to obtain the heat storage and heating filler nano powder.
Specifically, if the precursor xerogel is prepared by mixing and reacting the first solution corresponding to the ammonium tungstate with the second solution corresponding to the cesium bicarbonate, the precursor sol is dried at 100 ℃ for 6 hours to obtain the precursor xerogel, and then the precursor xerogel is annealed at 600 ℃ for 0.5 hour and naturally cooled to room temperature to obtain the heat storage and heating filler nanopowder.
Step S40, blending the heat storage and heating filler nano powder and polyester polymer, and granulating to obtain functional master batches;
and step S50, performing melt spinning on the functional master batch to obtain the energy storage heating fiber.
After the heat storage and heating filler nano powder is prepared, the heat storage and heating filler nano powder and polyester polymer are blended and fed in and out for granulation, to prepare the functional master batch, specifically, one or more of an open mill, an internal mixer, a single-screw extrusion granulator and a double-screw extrusion granulator are adopted to blend the heat storage and heat generation filler nano powder and the polyester polymer for in-out granulation, the polyester polymer comprises one or more of polyamide, methylcellulose, polyacrylonitrile, viscose cellulose, polymethyl methacrylate, polyester, cellulose acetate, polyolefin, polyvinyl alcohol, cuprammonium cellulose, polyurethane and polycarbonate, for example, polyacrylonitrile and the prepared energy storage heating filler are blended, extruded and granulated by a single-screw extrusion granulator to prepare functional master batches, and then the functional master batches are subjected to melt spinning to prepare the energy storage heating fiber.
Based on the first embodiment, a second embodiment of the method for preparing an energy storage and heat generation fiber according to the present invention is provided, in this embodiment, a characterization is performed on the prepared energy storage and heat generation fiber, and referring to fig. 2, fig. 2 is an X-ray diffraction diagram of an energy storage and heat generation fiber corresponding to tungsten tetrachloride and cesium chloride, specifically, in this embodiment, 20g of tungsten tetrachloride and 10g of polyvinylpyrrolidone are added to 75mL of deionized water to prepare a first solution, then 3.3g of cesium chloride and 1g of polyvinyl alcohol are added to 20mL of deionized water to prepare a second solution, then the second solution is dropped into the first solution at a speed of 1 drop/second to prepare a precursor sol, and then the precursor sol is dried at 100 ℃ for 12 hours to obtain a precursor xerogel, and the precursor xerogel is annealed at 500 ℃ for 1 hour to prepare a heat storage and heat generation filler nanopowder, and finally, blending the polyester polymer and the prepared heat storage and heating filler nano powder by a single-screw extrusion granulator, extruding and granulating to obtain functional master batches, and carrying out melt spinning on the functional master batches to obtain the product.
After the product is obtained, an X-ray diffraction pattern of the product is obtained by an X-ray diffractometer, as shown in FIG. 2, and is processed by a standard PDF cardComparing to obtain a product of Cs0.32WO3Thus, the product prepared in the example is the energy storage heating fiber Cs0.32WO3Further, the shape of the product was observed by a field emission scanning electron microscope, and as shown in fig. 3, it was found that the average particle size of the product was about 30nm and the size was uniform. Therefore, the heat storage and heating filler nano powder with the average particle size of 30nm and uniform size is successfully prepared in the embodiment 1 of the invention, and further, the infrared thermal imaging thermometer is utilized to detect the heating performance of the energy storage functional master batch and the common polymer prepared in the embodiment. As can be seen from fig. 4, the temperature of the energy storage functional masterbatch prepared in the embodiment of the present invention after being irradiated for 10 minutes can reach 55 degrees celsius, and compared with the common polymer, the energy storage functional masterbatch has a good light heating effect.
Based on the first and second embodiments, a third embodiment of an energy-storing and heat-generating fiber is provided, and the energy-storing and heat-generating fiber described in this embodiment is prepared by the energy-storing and heat-generating fiber preparation method described in the first and second embodiments.
Specifically, if the tungsten source is tungsten ethoxide and the cesium source is cesium carbonate, 33.8g of tungsten ethoxide and 5g of oxalic acid are added into 60mL of ethanol to prepare a first solution, 8g of cesium carbonate and 3g of L-cysteine are added into a mixed solvent of 15mL of ethanol and 15mL of deionized water to prepare a second solution, the second solution is dropwise added into the first solution at a speed of 2 drops/second to prepare a precursor sol, the precursor sol is dried at 75 ℃ for 6 hours to obtain a precursor xerogel, the precursor xerogel is annealed at 450 ℃ for 2 hours to prepare the energy storage heating filler, and finally the polypropylene polymer and the prepared energy storage heating filler are extruded, blended, extruded and granulated by twin screws to prepare the functional master batch. And performing melt spinning on the functional master batches to obtain the energy storage heating fiber corresponding to the tungsten ethoxide and the cesium carbonate.
If the tungsten source is sodium tungstate and the cesium source is cesium hydroxide, 25g of sodium tungstate and 8g L-cysteine are added into a mixed solvent of 15mL of ethanol and 60mL of deionized water to prepare a first solution, 4.7g of cesium hydroxide and 1.5g of oxalic acid are added into 20mL of deionized water to prepare a second solution, the second solution is dropwise added into the first solution at the speed of 1.5 drops/second to prepare a precursor sol, the precursor sol is dried for 10 hours at 80 ℃ to obtain a precursor xerogel, the precursor xerogel is annealed for 1 hour at 600 ℃ to prepare an energy storage heating filler, finally, the polypropylene polymer and the prepared energy storage heating filler are extruded and blended by a twin-screw extruder to prepare a functional master batch, and the functional master batch is melted to prepare the energy storage heating fiber corresponding to the sodium tungstate and the cesium hydroxide.
In this embodiment, the energy storage heating fiber prepared based on the preparation method of the energy storage heating fiber can effectively shield solar ultraviolet radiation, human body thermal radiation and absorb infrared thermal radiation, and has strong absorption function in a near infrared region and an ultraviolet region.
According to the scheme, a first solution is prepared by using a tungsten source and a first surfactant, a second solution is prepared by using a cesium source and a second surfactant, the first solution and the second solution are mixed to prepare a precursor sol, then the precursor sol is sequentially dried and annealed to prepare heat storage and heating filler nano powder, the heat storage and heating filler nano powder and a polyester polymer are mixed and fed in and out for granulation to prepare a functional master batch, and the functional master batch is subjected to melt spinning to prepare the energy storage and heating fiber.
It should be noted that, in this document, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or system that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or system. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method, article, or system that comprises the element.
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structures or flow transformations made by the present specification and drawings, or applied directly or indirectly to other related arts, are included in the scope of the present invention.
Claims (10)
1. The preparation method of the energy storage heating fiber is characterized by comprising the following steps of:
preparing a first solution by using a tungsten source and a first surfactant, and preparing a second solution by using a cesium source and a second surfactant;
mixing the first solution and the second solution to prepare a precursor sol;
drying and annealing the precursor sol in sequence to prepare heat storage and heating filler nano powder;
mixing the heat storage and heating filler nano powder with a polyester polymer, and granulating to obtain functional master batches;
and carrying out melt spinning on the functional master batch to prepare the energy storage heating fiber.
2. The method for preparing an energy-storing and heat-generating fiber according to claim 1, wherein the steps of preparing a first solution by using a tungsten source and a first surfactant and preparing a second solution by using a cesium source and a second surfactant comprise:
adding a tungsten source and a first surfactant into a first solvent, stirring and mixing to obtain a first solution;
the cesium source and the second surfactant are added to the second solvent and mixed with stirring to obtain a second solution.
3. The method for preparing an energy storage and heat emission fiber according to claim 2, wherein the molar ratio of tungsten element in the tungsten source and cesium element in the cesium source is greater than or equal to 2, the tungsten source comprises one or more of tungsten chloride, tungstic acid, tungsten carbonyl, sodium tungstate, ammonium tungstate and tungsten ethoxide, and the cesium source comprises one or more of cesium chloride, cesium formate, cesium hydroxide, cesium carbonate, cesium nitrate, cesium sulfate, cesium acetate, cesium bicarbonate and cesium amide.
4. The method for preparing energy-storage heating fiber according to claim 2, wherein the first surfactant and the second surfactant comprise one or more of lignosulfonate, heavy alkylbenzene sulfonate, alkylsulfonate, cetyl trimethyl ammonium bromide, sodium dodecylbenzene sulfonate, polyvinylpyrrolidone, polyvinyl alcohol, citric acid, oxalic acid, L-cysteine, disodium ethylenediamine tetraacetate, lauroyl glutamic acid, sodium stearyl sulfate and sodium fatty alcohol polyoxyethylene ether sulfate, wherein the first surfactant and the second surfactant are different.
5. The method for preparing an energy-storing and heat-generating fiber according to claim 2, wherein the first solvent and the second solvent comprise one or more of deionized water, cyclohexane, ethanol and acetone.
6. The method for preparing an energy-storing and heat-generating fiber according to claim 1, wherein the step of mixing the first solution and the second solution to obtain a precursor sol comprises:
and dripping the second solution into the first solution at a preset speed, and controlling the temperature of the first solution within a preset temperature range to prepare a precursor sol.
7. The method for preparing the energy-storage heating fiber according to claim 1, wherein the step of sequentially drying and annealing the precursor sol to prepare the heat-storage heating filler nano-powder comprises the following steps:
drying the precursor sol to obtain a precursor xerogel;
calcining the precursor xerogel at the temperature of between 300 and 1200 ℃ for 0.5 to 12 hours, and naturally cooling to room temperature to prepare the heat storage and heating filler nano powder.
8. The method for preparing energy-storage heating fiber according to claim 1, wherein the polyester polymer comprises one or more of polyamide, methylcellulose, polyacrylonitrile, viscose cellulose, polymethyl methacrylate, polyester, cellulose acetate, polyolefin, polyvinyl alcohol, cuprammonium cellulose, polyurethane and polycarbonate.
9. A method for preparing energy storage heating fiber according to any one of claims 1 to 8, wherein the heat storage heating filler nanopowder and the polyester macromolecule are blended and granulated in and out by one or more of an open mill, an internal mixer, a single screw extrusion granulator and a double screw extrusion granulator.
10. An energy-storage heating fiber, which is prepared by the preparation method of the energy-storage heating fiber of any one of claims 1 to 9.
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| CN109252402A (en) * | 2018-07-10 | 2019-01-22 | 长兴金发纺织有限公司 | A kind of low pollution dark color bedclothes fabric colouring method |
| CN112210844A (en) * | 2020-10-16 | 2021-01-12 | 中国科学技术大学先进技术研究院 | Composite silk and preparation method thereof |
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