WO2020137595A1 - Milieu chauffant liquide - Google Patents

Milieu chauffant liquide Download PDF

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Publication number
WO2020137595A1
WO2020137595A1 PCT/JP2019/048777 JP2019048777W WO2020137595A1 WO 2020137595 A1 WO2020137595 A1 WO 2020137595A1 JP 2019048777 W JP2019048777 W JP 2019048777W WO 2020137595 A1 WO2020137595 A1 WO 2020137595A1
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WO
WIPO (PCT)
Prior art keywords
fine particles
photothermal conversion
tungsten oxide
liquid
light
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PCT/JP2019/048777
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English (en)
Japanese (ja)
Inventor
裕史 常松
長南　武
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住友金属鉱山株式会社
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Priority to JP2020563072A priority Critical patent/JP7347446B2/ja
Publication of WO2020137595A1 publication Critical patent/WO2020137595A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
    • F24S70/00—Details of absorbing elements
    • F24S70/10—Details of absorbing elements characterised by the absorbing material
    • F24S70/16—Details of absorbing elements characterised by the absorbing material made of ceramic; made of concrete; made of natural stone
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24—HEATING; RANGES; VENTILATING
    • F24S—SOLAR HEAT COLLECTORS; SOLAR HEAT SYSTEMS
    • F24S80/00—Details, accessories or component parts of solar heat collectors not provided for in groups F24S10/00-F24S70/00
    • F24S80/20—Working fluids specially adapted for solar heat collectors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/40—Solar thermal energy, e.g. solar towers

Definitions

  • the present invention relates to a liquid heating medium.
  • the applicant of the present application discloses in Patent Document 1 that the infrared shielding material particles containing tungsten oxide fine particles and/or composite tungsten oxide fine particles have a particle diameter of 1 nm or more and 800 nm or less.
  • the infrared ray shielding material fine particle dispersion having excellent optical properties, such as shielding sunlight rays, particularly light in the near infrared region more efficiently, and at the same time maintaining the transmittance in the visible light region. It has been disclosed that can be prepared.
  • the infrared absorbing particles containing tungsten oxide or composite tungsten oxide have excellent photothermal conversion characteristics for converting the absorbed infrared rays into heat, and can be used for various applications utilizing these characteristics. Therefore, various studies have been made accordingly.
  • the applicant of the present application invented a light-absorbing resin composition for laser welding, which was stable in Patent Document 2, utilizing the characteristic that functional fine particles such as composite tungsten oxide absorb light to generate heat.
  • Patent Document 3 utilizes the characteristic that the functional fine particles such as composite tungsten oxide absorb light to generate heat, and thus the tungsten oxide particles and/or the composite tungsten oxide particles are
  • the inventors have invented a near-infrared absorbing fiber that is a fiber contained on the surface and/or inside, and a fiber product obtained by processing the near-infrared absorbing fiber, and disclosed a method for applying heat and heat.
  • ITO indium oxide
  • ATO antimony-doped tin oxide
  • hexaboride hexaboride
  • Patent Document 4 proposes a sunlight absorbing fluid in which titanium nitride is used as a material of the photothermal conversion fine particles, and titanium nitride nanoparticles capable of efficiently absorbing sunlight energy and heating the fluid are dispersed. There is.
  • the liquid heating medium is used to absorb the solar energy and transfer the heat to the device. Then, these liquid heating mediums are used by circulating them in a heating medium transfer facility such as a heat pump, a thermoelectric conversion element, and others (in the present invention, sometimes referred to as “heat pump etc.”). Is done.
  • a heating medium transfer facility such as a heat pump, a thermoelectric conversion element, and others (in the present invention, sometimes referred to as “heat pump etc.”).
  • a solar light absorbing fluid in which titanium nitride nanoparticles or the like as disclosed in Patent Document 4 is applied as a heating medium, the titanium nitride nanoparticles or the like have high hardness. Since the particles are particles, it has been found that there is a problem that a member of a heating medium conveying facility such as a heat pump is significantly worn and it is difficult to operate for a long period of time.
  • the present invention has been made under the above-mentioned circumstances, and the problem is that it has an infrared absorption property from sunlight, and the temperature of the temperature medium conveying facility is hardly worn and the temperature is not increased.
  • the purpose of the present invention is to provide a liquid heating medium that enables long-term operation of the medium transfer facility.
  • the inventors of the present invention have conducted research and as a result, have a combination of excellent visible light transmittance and infrared absorption characteristics, and a liquid temperature medium containing low hardness infrared absorption fine particles as photothermal conversion fine particles. And completed the present invention. That is, the invention for solving the above-mentioned problems is a liquid heating medium in which photothermal conversion fine particles that absorb sunlight energy or the like and convert it into heat are dispersed in a liquid medium.
  • FIG. 3 is a schematic diagram of a crystal structure of a composite tungsten oxide having a hexagonal crystal.
  • the heating medium according to the present invention is a liquid heating medium in which photothermal conversion fine particles that absorb light such as sunlight and convert it into heat are dispersed in the liquid medium.
  • the photothermal conversion fine particles are characterized by being tungsten oxide fine particles and/or composite tungsten oxide fine particles which are infrared absorbing fine particles.
  • the medium used for the liquid heating medium according to the present invention includes organic solvents, oils and fats, petroleum-derived media, liquid resins, liquid plasticizers for plastics, and polymerized by curing. It is possible to use one or more liquid media selected from the compounds, water and the like.
  • organic solvent it is possible to select various ones such as alcohol, ketone, hydrocarbon, glycol and water.
  • alcohol solvents such as methanol, ethanol, 1-propanol, isopropanol, butanol, pentanol, benzyl alcohol and diacetone alcohol; ketones such as acetone, methyl ethyl ketone, methyl propyl ketone, methyl isobutyl ketone, cyclohexanone and isophorone.
  • Ester solvent such as 3-methyl-methoxy-propionate; Ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol isopropyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol methyl ether acetate, propylene Glycol derivatives such as glycol ethyl ether acetate; amides such as formamide, N-methylformamide, dimethylformamide, dimethylacetamide, N-methyl-2-pyrrolidone; aromatic hydrocarbons such as toluene and xylene; ethylene chloride, Examples thereof include halogenated hydrocarbons such as chlorobenzene.
  • organic solvents having low polarity are preferable, and isopropyl alcohol, ethanol, 1-methoxy-2-propanol, dimethyl ketone, methyl ethyl ketone, methyl isobutyl ketone, toluene, propylene glycol monomethyl ether acetate, n-butyl acetate, etc. are more preferable. preferable.
  • These solvents may be used alone or in combination of two or more.
  • vegetable oils compounds derived from vegetable oils and the like can be used.
  • vegetable oil linseed oil, sunflower oil, tung oil, sesame oil, cottonseed oil, rapeseed oil, soybean oil, rice bran oil, olive oil, coconut oil, palm oil, dehydrated castor oil and the like are preferable.
  • compound derived from vegetable oil fatty acid monoester obtained by direct esterification reaction of fatty acid of vegetable oil and monoalcohol, ethers and the like are preferable.
  • petroleum-derived medium commercially available petroleum-based solvents and mineral oils can be used.
  • the petroleum solvent include Isopar E, Exol Hexane, Exol Heptane, Exol E, Exol D30, Exol D40, Exol D60, Exol D80, Exol D95, Exol D110, Exol D130 (above, manufactured by ExxonMobil) and the like.
  • the mineral oil are preferably paraffin-based and naphthene-based oils.
  • Liquid plasticizers for plastics include plasticizers that are compounds of monohydric alcohols and organic acid esters, ester-based plasticizers such as polyhydric alcohol organic acid ester compounds, and phosphorus such as organic phosphoric acid-based plasticizers.
  • a preferable example is an acid-based plasticizer.
  • triethylene glycol di-2-ethyl hexaonate, triethylene glycol di-2-ethyl butyrate, and tetraethylene glycol di-2-ethyl hexaonate are more preferable because they have low hydrolyzability.
  • Photothermal conversion fine particles used for liquid heating medium are tungsten oxide fine particles and/or composite tungsten oxide fine particles which are infrared absorbing fine particles.
  • tungsten oxide WO 3
  • absorption/reflection characteristics in the infrared region are small, and it is not effective as photothermal conversion fine particles.
  • WO 3 having oxygen deficiency and composite tungsten oxide obtained by adding a positive element such as Na to WO 3 are conductive materials and have free electrons. Analysis of single crystals of these materials having free electrons suggests the response of free electrons to light in the infrared region.
  • the present inventors have found that there is a particularly effective range as photothermal conversion fine particles in a specific portion of the composition range of the tungsten and oxygen. Then, it has been conceived that the tungsten oxide fine particles and the composite tungsten oxide fine particles which are transparent in the visible light region and have absorption in the infrared region are suitable as the photothermal conversion fine particles used for the liquid heating medium.
  • the hardness is considered to be low.
  • the tungsten oxide fine particles and the composite tungsten oxide fine particles are excellent photothermal conversion fine particles also from the viewpoint of enabling long-time operation without abrading members of equipment such as a heat pump. ..
  • tungsten oxide fine particles and/or the composite tungsten oxide fine particles which are the photothermal conversion fine particles according to the present invention
  • the composite tungsten oxide fine particles will be described in this order.
  • the tungsten oxide fine particle according to the present invention is a tungsten oxide represented by the general formula WyOz (where W is tungsten, O is oxygen, and 2.2 ⁇ z/y ⁇ 2.999). It is a fine particle.
  • the composition range of the tungsten and oxygen is such that the composition ratio of oxygen to tungsten is less than 3, and further, when the tungsten oxide fine particles are described as WyOz, 2 It is preferable that 0.2 ⁇ z/y ⁇ 2.999.
  • the value of x/y indicating the added amount of the element M will be described.
  • the value of x/y is larger than 0.001
  • a sufficient amount of free electrons are generated in the composite tungsten oxide, and the desired infrared absorption effect can be obtained.
  • the amount of the element M added increases, the supply amount of free electrons increases and the infrared absorption efficiency also increases, but the effect is saturated when the value of x/y is about 1.
  • the value of x/y is smaller than 1, it is possible to avoid generation of an impurity phase in the photothermal conversion fine particles, which is preferable.
  • the element M is H, He, alkali metal, alkaline earth metal, rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Au. , Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti, Nb, V, Mo, Ta, Re, Be. , Hf, Os, Bi, and I are preferably one or more.
  • the element M is an alkali metal, an alkaline earth metal, a rare earth element, Mg, Zr, Cr, Mn, Fe, Ru, Co, Rh, Ir. , Ni, Pd, Pt, Cu, Ag, Au, Zn, Cd, Al, Ga, In, Tl, Si, Ge, Sn, Pb, Sb, B, F, P, S, Se, Br, Te, Ti More preferably, it is one or more kinds of elements selected from Nb, V, Mo, Ta, and Re. From the viewpoint of improving the optical characteristics and weather resistance of the photothermal conversion fine particles, the element M more preferably belongs to the alkaline earth metal elements, transition metal elements, 4B group elements, and 5B group elements.
  • the composite tungsten oxide fine particles have a hexagonal crystal structure
  • the transmission of the fine particles in the visible light region is improved and the absorption in the infrared region is improved. This will be described with reference to FIG. 1, which is a schematic plan view of the crystal structure of this hexagonal crystal.
  • the composite tungsten oxide fine particles contain the unit structure described with reference to FIG.
  • the composite tungsten oxide fine particles may be crystalline or amorphous.
  • the hexagonal crystal is likely to be formed. Specifically, hexagonal crystals are easily formed when Cs, K, Rb, Tl, In, Ba, Li, Ca, Sr, Fe and Sn are added.
  • other elements may be used as long as the above-mentioned element M exists in the hexagonal void formed by the WO 6 unit, and the elements are not limited to the above-mentioned elements.
  • the addition amount of the additional element M is preferably 0.2 or more and 0.5 or less, more preferably 0 or less in x/y value. .33.
  • the value of x/y is 0.33, it is considered that the element M described above is arranged in all the hexagonal voids.
  • tetragonal and cubic composite tungsten oxides are also effective as photothermal conversion fine particles.
  • the absorption position in the infrared region tends to change, and the absorption position tends to move to the longer wavelength side in the order of cubic crystal ⁇ tetragonal crystal ⁇ hexagonal crystal.
  • incidental low absorption in the visible light region is in the order of hexagonal crystal, tetragonal crystal, and cubic crystal. Therefore, it is preferable to use a hexagonal composite tungsten oxide for the purpose of transmitting light in the visible light region and absorbing light in the infrared light region.
  • the tendency of the optical characteristics described here is only a rough tendency and changes depending on the type of the added element, the added amount, and the oxygen amount, and the present invention is not limited to this.
  • Tungsten Oxide Fine Particles and Composite Tungsten Oxide Fine Particles The photothermal conversion fine particles containing the tungsten oxide fine particles and the composite tungsten oxide fine particles according to the present invention largely absorb light in the near infrared region, particularly in the vicinity of a wavelength of 1000 nm. Therefore, the transmitted color tone is often blue to green.
  • the so-called “Magneli phase” having a composition ratio represented by 2.45 ⁇ z/y ⁇ 2.999 is chemically stable, and is in the infrared region. Since it has good absorption characteristics, it is preferable as the photothermal conversion fine particles.
  • the crystallite diameter of the photothermal conversion fine particles is preferably 1 nm or more and 200 nm or less, more preferably 1 nm or more and 100 nm or less, and further preferably 10 nm or more and 70 nm or less.
  • measurement of an X-ray diffraction pattern by a powder X-ray diffraction method ( ⁇ -2 ⁇ method) and analysis by the Rietveld method are used.
  • the X-ray diffraction pattern can be measured using, for example, a powder X-ray diffractometer "X'Pert-PRO/MPD" manufactured by Spectris KK PAnalytical.
  • the surface of the photothermal conversion fine particles according to the present invention is coated with an oxide containing one or more kinds of metals of Si, Ti, Zr, Al and Zn from the viewpoint of improving weather resistance.
  • the coating method is not particularly limited, but it is possible to coat the surface of the photothermal conversion fine particles by adding the metal alkoxide to the solution in which the photothermal conversion fine particles are dispersed.
  • a dispersant such as a coupling agent, and a surfactant may be added to the liquid heating medium according to the present invention.
  • the dispersant, the coupling agent, and the surfactant can be selected according to the application, but preferably have an amine-containing group, a hydroxyl group, a carboxyl group, or an epoxy group as a functional group. These functional groups are adsorbed on the surface of the tungsten oxide fine particles or the composite tungsten oxide fine particles, prevent the aggregation of the tungsten oxide fine particles or the composite tungsten oxide fine particles, and make the photothermal conversion fine particles according to the present invention uniform in the heating medium. Has the effect of being dispersed.
  • Suitable dispersants include, but are not limited to, phosphate ester compounds, polymer dispersants, silane coupling agents, titanate coupling agents, aluminum coupling agents, and the like. Not a thing.
  • the polymer dispersant include an acrylic polymer dispersant, a urethane polymer dispersant, an acrylic/block copolymer polymer dispersant, a polyether dispersant, and a polyester polymer dispersant.
  • the liquid heating medium according to the present invention absorbs sunlight energy and the like and converts it into heat, and enables long-time operation without abrading the members of the equipment. Is. Therefore, it is suitable as a heating medium for a heat pump or the like using solar energy or the like.
  • the crystallite size of the photothermal conversion fine particles in the dispersions according to the examples, comparative examples and reference examples was measured by powder X-ray diffractometry using a powder X-ray diffractometer (Spectris Co., Ltd. PANalytical X'Pert-PRO/MPD). ( ⁇ 2 ⁇ method), and calculated using Rietveld method.
  • the optical characteristics of the photothermal conversion microparticles were measured using a spectrophotometer (U-4100 manufactured by Hitachi, Ltd.) by placing the diluted photothermal conversion microparticle dispersion in a measuring glass cell with a light path of 20 mm.
  • the visible light transmittance and the solar radiation transmittance were calculated according to JISR3106.
  • the incident direction of the light of the spectrophotometer was perpendicular to the measuring glass cell.
  • a blank liquid in which only pure water as a main solvent was put in the measurement glass cell was used as a baseline of light transmittance.
  • the light-heat conversion fine particles dispersion is diluted to a visible light transmittance of 70%, and the solar light approximate spectrum lamp (SAN-EI ELECTRIC solar simulator is used from the initial state at a liquid temperature of 23° C.).
  • SAN-EI ELECTRIC solar simulator is used from the initial state at a liquid temperature of 23° C.
  • XES-40S1 is used to irradiate artificial sunlight corresponding to AM (Air Mass) 1.5 at a radiant intensity of light of 1500 W/m 2 for 20 minutes to measure the temperature rise range of the photothermal conversion fine particle dispersion before and after irradiation. did.
  • the room temperature at this time was 23°C.
  • a composite tungsten oxide powder (YM-01 manufactured by Sumitomo Metal Mining Co., Ltd.) containing ⁇ 3.0) was prepared. Then, the mixed solution obtained by mixing 20% by mass of the photothermal conversion material and 80% by mass of pure water was loaded into a paint shaker containing 0.3 mm ⁇ ZrO 2 beads and pulverized and dispersed for 20 hours, A photothermal conversion fine particle dispersion liquid of Cs 0.33 WOz was obtained.
  • the crystallite diameter of the photothermal conversion fine particle was measured and found to be 23 nm. The measurement results are shown in Table 1.
  • the obtained light-heat conversion fine particle dispersion was diluted with pure water until the concentration of the light-heat conversion fine particles became 0.023% by mass to obtain the light-heat conversion fine particle dispersion according to Example 1.
  • the visible light transmittance was 49% and the solar radiation transmittance was 19%.
  • Example 2 and 3 The light-heat converting fine particle dispersion liquid described in Example 1 was diluted with pure water until the concentration of the light-heat converting fine particles became 0.0023% by mass to obtain the light-heat converting fine particle dispersion liquid according to the second embodiment. The mixture was diluted with pure water to 0.00023% by mass to obtain a photothermal conversion fine particle dispersion liquid according to Example 3. Then, in the same manner as in Example 1, the optical characteristics of the photothermal conversion fine particle dispersion liquids according to Examples 2 and 3 were measured. The measurement results are shown in Table 1.
  • Comparative Example 1 As a comparative example, pure water was used as the light-heat converting fine particle dispersion liquid, and the optical characteristics of the light-heat converting fine particle dispersion liquid according to the first comparative example were measured in the same manner as in Example 1. The range of increase was 6.9°C. The measurement results are shown in Table 1.
  • the photothermal conversion material was changed from the composite tungsten oxide powder to tin-doped indium oxide (ITO) powder to obtain photothermal conversion fine particle dispersions according to Reference Examples 1 to 4.
  • the light-heat conversion fine particle dispersion liquid according to Reference Example 1 was obtained by setting the concentration of light-heat conversion fine particles at the time of optical characteristic measurement to 0.071 mass %, and the concentration was 0.050 mass%, and the light-heat conversion fine particle dispersion liquid according to Reference Example 2 was obtained.
  • a concentration of 0.0071 mass% to obtain a photothermal conversion fine particle dispersion according to Reference Example 3 and a concentration of 0.00071 mass% to obtain a photothermal conversion fine particle dispersion according to Reference Example 4.
  • the light-heat conversion material was changed from the composite tungsten oxide powder to the antimony-doped tin oxide (ATO) powder to obtain the light-heat conversion fine particle dispersions according to Reference Examples 5 to 8.
  • the light-heat conversion fine particle dispersion liquid according to Reference Example 5 was obtained by setting the concentration of the light-heat conversion fine particles at the time of optical property measurement to 0.099 mass%, and the concentration was 0.066 mass%, and the light-heat conversion fine particle dispersion liquid according to Reference Example 6 was obtained.
  • a photothermal conversion fine particle dispersion according to Reference Example 7 with a concentration of 0.0066% by mass and obtain a photothermal conversion fine particle dispersion according to Reference Example 8 with a concentration of 0.00066% by mass.
  • the light-heat conversion material was changed from the composite tungsten oxide powder to the titanium nitride powder to obtain light-heat conversion fine particle dispersions according to Reference Examples 11 and 12.
  • the light-heat conversion fine particle dispersion liquid according to Reference Example 11 was obtained by setting the concentration of the light-heat conversion fine particles at the time of optical characteristic measurement to 0.00061% by mass, and the concentration was 0.00052% by mass, and the light-heat conversion fine particle dispersion liquid according to Reference Example 12 was obtained.

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Abstract

L'invention concerne un milieu chauffant liquide dans lequel sont dispersées des microparticules de conversion photothermique qui absorbent la lumière et convertissent la lumière absorbée en chaleur.
PCT/JP2019/048777 2018-12-27 2019-12-12 Milieu chauffant liquide WO2020137595A1 (fr)

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JP2020563072A JP7347446B2 (ja) 2018-12-27 2019-12-12 液状の温媒

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JP2018244227 2018-12-27
JP2018-244227 2018-12-27

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WO2020137595A1 true WO2020137595A1 (fr) 2020-07-02

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006049025A1 (fr) * 2004-11-08 2006-05-11 Sumitomo Metal Mining Co., Ltd. Fibre absorbant le rayonnement infrarouge proche et produit textile utilisant celle-ci
JP2010144957A (ja) * 2008-12-16 2010-07-01 Ihi Corp 太陽熱集熱方法及び装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006049025A1 (fr) * 2004-11-08 2006-05-11 Sumitomo Metal Mining Co., Ltd. Fibre absorbant le rayonnement infrarouge proche et produit textile utilisant celle-ci
JP2010144957A (ja) * 2008-12-16 2010-07-01 Ihi Corp 太陽熱集熱方法及び装置

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JPWO2020137595A1 (ja) 2021-11-18
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