CN118835095A - Method for dissolving noble metal by photocatalysis - Google Patents
Method for dissolving noble metal by photocatalysis Download PDFInfo
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- CN118835095A CN118835095A CN202410893210.1A CN202410893210A CN118835095A CN 118835095 A CN118835095 A CN 118835095A CN 202410893210 A CN202410893210 A CN 202410893210A CN 118835095 A CN118835095 A CN 118835095A
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- 229910000510 noble metal Inorganic materials 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 19
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 11
- 238000004090 dissolution Methods 0.000 claims abstract description 44
- 239000011941 photocatalyst Substances 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- 150000002825 nitriles Chemical class 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical group CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 51
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical group ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 27
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 4
- 239000010931 gold Substances 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052741 iridium Inorganic materials 0.000 claims description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 2
- 239000011133 lead Substances 0.000 claims description 2
- 229910052762 osmium Inorganic materials 0.000 claims description 2
- SYQBFIAQOQZEGI-UHFFFAOYSA-N osmium atom Chemical compound [Os] SYQBFIAQOQZEGI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 238000011084 recovery Methods 0.000 abstract description 13
- 239000000460 chlorine Substances 0.000 abstract description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000004134 energy conservation Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 30
- 238000006243 chemical reaction Methods 0.000 description 11
- DEZRYPDIMOWBDS-UHFFFAOYSA-N dcm dichloromethane Chemical compound ClCCl.ClCCl DEZRYPDIMOWBDS-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 150000003839 salts Chemical class 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 4
- 230000008020 evaporation Effects 0.000 description 4
- 239000010970 precious metal Substances 0.000 description 4
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910052720 vanadium Inorganic materials 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000005065 mining Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000006864 oxidative decomposition reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
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- 239000002341 toxic gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention provides a method for dissolving noble metals by photocatalysis, and belongs to the technical field of noble metal recovery. The method provided by the invention is that a sample containing noble metal and a photocatalyst are added into a mixed solution containing organic nitrile and organic chlorine, and the metal can be dissolved after light irradiation for a certain time. The invention provides a brand-new idea for improving the green dissolution and recovery of noble metals, and the whole process has the advantages of mildness, energy conservation, greenness, environmental protection, low cost, convenient operation and the like, and can realize the efficient recovery of noble metals under the environment-friendly and mild conditions without consuming excessive energy sources only by introducing the photocatalysis technology.
Description
Technical Field
The invention relates to the technical field of precious metal recovery, in particular to a method for dissolving precious metal by photocatalysis.
Background
Noble metals are very popular for use in production and life, and are very important industrial raw materials in modern industry. However, noble metals have limited resources, and excessive exploitation and smelting not only bring adverse effects to the environment, but also occupy 7% -8% of the energy supply worldwide. The recovery of precious metals consumes less energy than primary mining while reducing the overall impact on the mineral mining site. However, precious metal recovery is still maintained at a low level, subject to process and recovery costs.
The existing noble metal extraction method mainly comprises a chemical method and an electrolytic method, wherein the electrolytic method is to utilize a cathode column to adsorb noble metal elements for recovery, but in the electrolytic process, along with the increase of the noble metal elements adsorbed by the cathode column, the adsorption capacity of the cathode column to the noble metal is gradually reduced, and the residual electrolyte can only be discharged for secondary electrolysis, so that the whole operation is complicated and the recovery efficiency is low. The process of dissolving noble metal with aqua regia and strong acid mixture includes the steps of using hydrochloric acid as complexing agent, using nitric acid, chlorine or hydrogen peroxide as oxidant and forming coordination complex with noble metal to recover noble metal. However, this technique cannot avoid the use and post-treatment of strong acids, which is a serious hazard to the environment and the operators of use. The recovery of noble metals by electrolysis is usually carried out by substitution reaction of noble metals with other active metals, and is usually accompanied by a temperature raising operation for increasing the reaction rate, thereby achieving the purpose of recovering noble metals. However, such methods consume electrical energy continuously, which is not beneficial to sustainable development of energy.
Disclosure of Invention
In view of the above, the invention provides a method for dissolving noble metals by photocatalysis, which can realize the efficient recovery of noble metals under the environment-friendly and mild conditions.
In order to achieve the above object, the present invention provides the following technical solutions: a method for dissolving noble metal by photocatalysis includes such steps as adding the sample containing noble metal and photocatalyst to the mixed solution containing organic nitrile and organic chloride, and light irradiation for a certain time.
In some embodiments, the noble metal comprises one or more of osmium, ruthenium, rhodium, iridium, gold, silver, platinum, palladium, copper, or lead.
In some embodiments, the photocatalyst is an inorganic photocatalyst.
In some embodiments, the inorganic photocatalyst is TiO 2.
In some embodiments, the organic nitrile is acetonitrile.
In some embodiments, the organochlorine is methylene chloride.
In some embodiments, the volume ratio of organonitrile to organochlorine is (0.1-10): 1.
In some embodiments, the light is illuminated at a wavelength of 150-1500nm, covering deep ultraviolet light, visible light, and near infrared light.
The principle of the photocatalytic dissolving of noble metals in the invention is as follows:
In the whole dissolution system, besides light and a photocatalyst are indispensable factors, the property of a solvent is also crucial, and cyano (-CN) and organic chlorine (-Cl) in the combination of acetonitrile and dichloromethane are key to the success of the dissolution reaction. Under the excitation of light, the photocatalyst TiO 2 generates electrons and holes; electrons generated by light excitation react with O 2 molecules to generate O 2 -, and holes react with CH 3 CN in the mixed solvent to generate CHCN free radicals; oxidative decomposition of CH 2Cl2 to CH 2 Cl radicals; oxidation of PM 0 to PM x+ form (NH 4) xPMCly solid by active species synergy; finally, the obtained noble metal solid salt is roasted to obtain high-purity noble metal.
The invention discloses the following technical effects:
1. The invention provides a brand-new idea for improving the green dissolution and recovery of noble metals, and the whole process has the advantages of mildness, energy conservation, green, environmental protection, low cost, convenient operation and the like, and only needs to introduce a photocatalysis technology without consuming excessive energy sources.
2. The method for dissolving the noble metal by photocatalysis provided by the invention avoids the use and aftertreatment of strong acid, and is more environment-friendly.
3. The method for dissolving the noble metal by photocatalysis provided by the invention can realize the efficient recovery of the noble metal under the environment-friendly and mild conditions.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the time-dependent dissolution rate of example 1.
FIG. 2 is a scanning electron microscope image of the bulk electron CPU material before dissolution in example 3.
FIG. 3 is a graph showing the dissolution data of noble metals in bulk electronic CPU material in example 3.
Fig. 4 is a comparison of the electronic CPU material and the ore before and after dissolution in example 7, where a is a photograph of the electronic CPU material before dissolution, b is a photograph of the electronic CPU material after dissolution, c is a photograph of the ore before dissolution, and d is a photograph of the ore after dissolution.
Fig. 5 is an appearance of the electronic CPU material before and after dissolution in comparative example 1, where a is a photograph of the electronic CPU material before dissolution and b is a photograph of the electronic CPU material after dissolution.
Detailed Description
Various exemplary embodiments of the invention will now be described in detail, which should not be considered as limiting the invention, but rather as more detailed descriptions of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. In addition, for numerical ranges in this disclosure, it is understood that each intermediate value between the upper and lower limits of the ranges is also specifically disclosed. Every smaller range between any stated value or stated range, and any other stated value or intermediate value within the stated range, is also encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the invention described herein without departing from the scope or spirit of the invention. Other embodiments will be apparent to those skilled in the art from consideration of the specification of the present invention. The specification and examples of the present invention are exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are intended to be inclusive and mean an inclusion, but not limited to.
For a better understanding of the present invention, the following examples are further illustrated, but are not limited to the following examples.
The raw materials and reagents used in the examples were all obtained from commercial sources.
In the embodiment, the dissolution reaction is carried out in the condensing device, so that the pollution caused by volatilization of acetonitrile and dichloromethane to the environment is avoided, meanwhile, the condensing device is adopted to recycle the acetonitrile and the dichloromethane, the solvent can be recycled for more than 10 times, and the dissolution rate of noble metals is basically similar.
In an embodiment, the dissolution process is as follows:
(1) Dissolving: and pumping the solvent into a reaction kettle through a peristaltic pump, feeding the waste sample into the reaction kettle at one time, and dissolving out the materials under the irradiation of ultraviolet light/visible light. The reaction process is continuously stirred, the raw material liquid is gradually changed from colorless to light yellow, then gradually changed into golden yellow, and the noble metal is successfully dissolved in the raw material liquid.
(2) And (3) evaporation: the raw material liquid is separated and flows into the evaporation reaction kettle through a solid-liquid separation technology, a heating device is started to continuously glow the liquid, steam is condensed by a condensing pipe and then flows back to become colorless liquid, and the colorless liquid is collected in a collecting bottle and is further conveyed into the dissolution reaction kettle through a pump for recycling. Finally, only golden yellow solid salt is left in the evaporation reaction kettle, and the lifting device is started to take out the golden yellow solid salt.
(3) Roasting: and taking out the yellow solid salt obtained after evaporation, sending the yellow solid salt to a baking device unit, and heating to 500 ℃ in the atmosphere of hydrogen-argon mixed gas to finally obtain the high-purity noble metal solid.
Example 1
50Mg of ultra-low noble metal-loaded material (the loading of noble metal is 0.01-0.05wt%, and the noble metal comprises Ag, au, pt and Pd), and 50mg of titanium dioxide are added into a mixed solution of acetonitrile and dichloromethane (V Acetonitrile :V Dichloromethane (dichloromethane) = 2:7, wherein the mixed solution of acetonitrile and dichloromethane can submerge the ultra-low noble metal-loaded material), after the ultra-low noble metal-loaded material is irradiated by ultraviolet light for 4 hours, the solution is centrifuged, and the leaching amount of the noble metal in the solution is tested. The dissolution rate of noble metals in the solution before and after ICP detection reaction is close to 100 percent (95% -99%). The change rule of the dissolution rate with time is shown in figure 1.
Example 2
The difference from example 1 was only that the ultra-low noble metal-loaded material was replaced with a centimeter-sized bulk electronic CPU material (1 cm. Times.1 cm), a millimeter-sized bulk electronic CPU material (1 mm. Times.1 mm), and a micrometer-sized bulk electronic CPU material (1 μm. Times.1 μm), respectively.
The scanning electron microscope of the block electronic CPU material before dissolution is shown in figure 2, and it can be seen that the metal Cu, ni, ag, au is distributed on the CPU board. The dissolution data of the bulk noble metal is shown in figure 3. The results showed that the dissolution rates were all close to 100% (95% -99%).
Example 3
The only difference from example 1 is that the ultra low noble metal loading material was replaced with ore and the dissolution rate of noble metal in the ore was tested. The results showed that the dissolution rate was close to 100%.
Example 4
The only difference from example 1 is that V Acetonitrile :V Dichloromethane (dichloromethane) =2:7 is replaced by V Acetonitrile :V Dichloromethane (dichloromethane) =1:10. The dissolution rate of noble metals was tested. The results showed that the dissolution rate was close to 100%.
Example 5
The only difference from example 1 is that V Acetonitrile :V Dichloromethane (dichloromethane) =2:7 is replaced by V Acetonitrile :V Dichloromethane (dichloromethane) =10:1. The dissolution rate of noble metals was tested. The results showed that the dissolution rate was close to 100%.
Example 6
The only difference from example 1 is that V Acetonitrile :V Dichloromethane (dichloromethane) =2:7 is replaced by V Acetonitrile :V Dichloromethane (dichloromethane) =1:1. The dissolution rate of noble metals was tested. The results showed that the dissolution rate was close to 100%.
Example 7
This example demonstrates the dissolution effect of kg-scale electronic CPU material (1.137 kg) and ore (1.169 kg), and the dissolution process is the same as that of example 1. When the dissolution time was detected to be 12 hours, 18.3 mg and 26.1 mg of gold were dissolved from the CPU board and ore, respectively. After the dissolution time was prolonged to 48 hours, 32.5 mg and 65.9 mg of gold were captured, respectively. The comparison of the electronic CPU material and the ore before and after dissolution is shown in FIG. 4.
Comparative example 1
Uniformly mixing 1.137kg of electronic CPU material with aqua regia (the amount of the aqua regia can be enough to submerge the electronic CPU material), and standing for 4 hours for reaction. The appearance of the dissolved electronic CPU material was observed.
1.137Kg of an electronic CPU material, 50g of titanium dioxide light were added to a mixed solution of acetonitrile and methylene chloride (V Acetonitrile :V Dichloromethane (dichloromethane) = 2:7, the mixed solution of acetonitrile and methylene chloride was able to submerge the electronic CPU material), and irradiated with ultraviolet light for 4 hours. The appearance of the dissolved electronic CPU material was observed. The results are shown in FIG. 5. Compared with the aqua regia method with higher efficiency in the prior art, the aqua regia is reacted vigorously to generate toxic gases such as nitric oxide and chlorine and crack a CPU board, and the dissolved CPU material is cleaner and more thorough, safer and more environment-friendly and has extremely high competitiveness.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (8)
1. A method for dissolving noble metal by photocatalysis is characterized in that a sample containing noble metal and a photocatalyst are added into a mixed solution containing organic nitrile and organic chloride, and the metal can be dissolved by light irradiation for a certain time.
2. The method of photocatalytic dissolution of a noble metal according to claim 1, wherein the noble metal comprises one or more of osmium, ruthenium, rhodium, iridium, gold, silver, platinum, palladium, copper, and lead.
3. The method of photocatalytic dissolution of noble metals as set forth in claim 1, wherein the photocatalyst is an inorganic photocatalyst.
4. The method for photocatalytic dissolution of noble metals as set forth in claim 3, the method is characterized in that the inorganic photocatalyst is TiO 2.
5. The method of photocatalytic dissolution of noble metals according to claim 1, wherein the organic nitrile is acetonitrile.
6. The method for photocatalytic dissolution of noble metals according to claim 1, wherein the organochlorine is methylene chloride.
7. The method for photocatalytic dissolution of noble metals according to claim 1, wherein the volume ratio of the organic nitrile to the organic chloride is (0.1-10): 1.
8. The method for photocatalytic dissolution of noble metals according to claim 1, wherein the light irradiation has a wavelength of 150 to 1500nm, covering deep ultraviolet light, visible light and near infrared light.
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