CN116120775A - Cesium tungsten bronze slurry and preparation method and application thereof - Google Patents
Cesium tungsten bronze slurry and preparation method and application thereof Download PDFInfo
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- CN116120775A CN116120775A CN202211718534.9A CN202211718534A CN116120775A CN 116120775 A CN116120775 A CN 116120775A CN 202211718534 A CN202211718534 A CN 202211718534A CN 116120775 A CN116120775 A CN 116120775A
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- cesium tungsten
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- OHUPZDRTZNMIJI-UHFFFAOYSA-N [Cs].[W] Chemical compound [Cs].[W] OHUPZDRTZNMIJI-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 229910000906 Bronze Inorganic materials 0.000 title claims abstract description 101
- 239000010974 bronze Substances 0.000 title claims abstract description 101
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000002002 slurry Substances 0.000 title claims abstract description 96
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 238000007613 slurry method Methods 0.000 title description 2
- 239000002904 solvent Substances 0.000 claims abstract description 49
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 47
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 45
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 12
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims abstract description 6
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000000498 ball milling Methods 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 16
- 238000000227 grinding Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011324 bead Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 229920001451 polypropylene glycol Polymers 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 239000000314 lubricant Substances 0.000 claims description 4
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 2
- 229940057847 polyethylene glycol 600 Drugs 0.000 claims description 2
- 239000011810 insulating material Substances 0.000 claims 1
- 238000009413 insulation Methods 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 8
- 239000003960 organic solvent Substances 0.000 abstract description 6
- 238000002834 transmittance Methods 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 5
- 230000004048 modification Effects 0.000 abstract description 5
- 238000000576 coating method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000011248 coating agent Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 7
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 2
- 239000002346 layers by function Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011164 primary particle Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- MUGSTXRSLGJVOB-UHFFFAOYSA-N 2-[2-[2-(6-methylheptanoyloxy)ethoxy]ethoxy]ethyl 6-methylheptanoate Chemical compound C(CCCCC(C)C)(=O)OCCOCCOCCOC(CCCCC(C)C)=O MUGSTXRSLGJVOB-UHFFFAOYSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000005328 architectural glass Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- -1 cesium tungsten cyanCopper Chemical compound 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000005340 laminated glass Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000005344 low-emissivity glass Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/66—Additives characterised by particle size
- C09D7/67—Particle size smaller than 100 nm
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
Abstract
The invention discloses cesium tungsten bronze slurry and a preparation method and application thereof. The cesium tungsten bronze slurry has a particle size of 100nm or less and comprises any one of the following combinations: and (3) a step of: cesium tungsten bronze slurry includes the following: 10-40 parts of cesium tungsten bronze powder; 50-90 parts of a solvent; 1-10 parts of an auxiliary agent; the solvent comprises one or more of toluene, methyl isobutyl ketone, isopropanol and ethanol; the auxiliary agent comprises BYK2070; and II: cesium tungsten bronze slurry includes the following: 10-40 parts of cesium tungsten bronze powder; 50-90 parts of a solvent; 1-10 parts of an auxiliary agent; auxiliaries include BYK2070, BYK7410 and TEGO245. The cesium tungsten bronze powder in the cesium tungsten bronze slurry can be uniformly dispersed in an organic solvent, and the preparation method is simple, the modification of the cesium tungsten bronze powder is not needed, and the prepared cesium tungsten bronze slurry has good stability, good infrared heat insulation effect and high light transmittance.
Description
Technical Field
The invention relates to cesium tungsten bronze slurry and a preparation method and application thereof.
Background
The PVB, PET and other resins have chemical properties of being insoluble in water and soluble in benzene, esters, ketones and other organic solvents. In general, PVB and PET resins have good transparency, good light resistance, heat resistance, cold resistance, water resistance, film forming property, high tensile strength and impact resistance, no toxicity, good safety, good binding force with metals, glass, wood, ceramics, fiber products and the like, so the PVB and PET resins are widely applied and rapidly developed in the aspects of manufacturing safety laminated glass, paint, adhesives and the like.
In summer, in China, hot weather with temperature higher than 35 ℃ often occurs, and strong solar radiation can lead the internal temperature of a building or a vehicle which is a relatively closed space to be increased drastically, so that the ageing and degradation processes of indoor furniture, vehicle leather and plastic products are aggravated. However, conventional architectural glass lacks the ability to insulate, and in particular, the ability to insulate infrared radiation. In addition, the building energy consumption is counted to be larger in proportion of the total social energy consumption at present, and the tendency of annual increase is shown. The above situation causes a heavy energy burden and serious environmental pollution to society, so the development of a novel thermal-insulation coating has become a great trend of energy saving and emission reduction.
At present, the conventional heat shielding functional materials commonly used for transparent heat insulation are Low emissivity glass (Low-e), indium or antimony doped tin oxide (ITO or ATO) and nanometer LaB 6 . However, these materials currently still have some significant drawbacks. For example: the Low-e core Low-emissivity coating is a precious metal silver functional layer that exhibits solar heat reflection, and generally requires a complex coating structure and multiple functional layers, and places relatively high demands on the process and equipment. The ITO or ATO-based coatings also exhibit heat shielding capabilities; indium is an expensive rare metal resource, however, resulting in higher application costs. ATO has heat insulation effect mainly in the infrared band after reflecting 1500nm, has limited heat insulation effect, and has higher transmittance in the wavelength range of 780-1500 nm. The shielding capability of lanthanum hexaboride is particularly expressed in a wave band of about 1000nm, and a better method for preparing nanoscale lanthanum hexaboride in large quantity is not available at present, so that the production period and the cost are high.
The tungsten bronze transparent nano heat-insulating coating is characterized by environmental friendliness and high heat insulation, and particularly the cesium tungsten bronze transparent nano heat-insulating coating is distinguished from a plurality of transparent heat-insulating coatings. In general, the cesium tungsten bronze transparent nano heat insulation coating has higher surface activity and adsorptivity, aggregation is easy to occur, and the viscosity of the resin is generally higher, so that the cesium tungsten bronze transparent nano heat insulation coating is difficult to disperse, and if the cesium tungsten bronze transparent nano heat insulation coating cannot be uniformly dispersed in the resin, the property of absorbing infrared rays is lost. Therefore, cesium tungsten bronze nano-split bodies are required to be pre-dispersed into slurry, and then the slurry is added into resin to prepare the coating, and the preparation of the nano-slurry is one of key factors for successful preparation of the glass heat insulation coating. For example, chinese patent CN112552733A proposes cesium tungsten bronze aqueous slurry and a preparation method thereof, but the aqueous slurry is difficult to have good adhesive force on the surface of a PET substrate, and is particularly applied to an optical transparent PET film, and the surface is smooth and difficult to adhere. For another example, chinese patent CN107513293a proposes a preparation method of cesium tungsten bronze modified powder slurry: 1. placing cesium tungsten bronze powder in deionized water, dropwise adding acetic acid to adjust the pH value, sequentially adding a coupling agent, an infrared absorbent and an ultraviolet absorbent with the reaction amount to carry out surface treatment on the cesium tungsten bronze powder, stirring and reacting for 30 minutes, filtering to obtain powder subjected to surface treatment, and then placing the powder in a freeze dryer at the temperature of minus 40 ℃ to quickly freeze and sublimate and remove water to obtain cesium tungsten bronze modified powder; 2. adding the cesium tungsten bronze modified powder, the wetting dispersant and the triethylene glycol di-isooctanoate into a zirconia ball mill, wherein the diameter of zirconium beads is 0.1-0.3mm, the ball milling rotating speed is 1500rpm, the ball milling temperature is 25 ℃, and the ball milling is carried out for 8 hours, so that the cesium tungsten bronze modified powder slurry is obtained. The disadvantages of this are: 1. the dispersion medium adopts oily organic solvent, has long volatilization time and is not environment-friendly; 2. the process is complex, the nano powder is required to be modified, and the cesium tungsten bronze powder is insoluble in water, so that the modification efficiency is low; 3. the equipment requirement is high, and a freeze dryer is needed. The hydroxyl groups are taken as the main groups on the surface of cesium tungsten bronze, so that the cesium tungsten bronze shows stronger hydrophilicity, is difficult to uniformly disperse in an organic solvent, can cause layering difference, and affects the coating or film required subsequently.
Disclosure of Invention
The invention provides cesium tungsten bronze slurry and a preparation method and application thereof, and aims to overcome the defects that cesium tungsten bronze powder is difficult to disperse in an organic solvent, modification is needed when cesium tungsten bronze slurry is prepared, modification efficiency is low, procedures are complex, stability of the obtained cesium tungsten bronze slurry is poor and the like in the prior art. In the cesium tungsten bronze slurry, cesium tungsten bronze powder can be uniformly dispersed in an organic solvent, the preparation method is simple in procedure, modification of the cesium tungsten bronze powder is not needed, and the prepared cesium tungsten bronze slurry is good in stability and has the advantages of good infrared heat insulation effect, high light transmittance and the like.
The invention provides cesium tungsten bronze slurry, which comprises any one of the following combinations:
combining: the cesium tungsten bronze slurry comprises the following components in parts by weight:
cesium tungsten bronze powder: 10-40 parts of a lubricant; solvent: 50-90 parts; auxiliary agent: 1-10 parts;
wherein the solvent comprises one or more of toluene, methyl isobutyl ketone, isopropanol and ethanol; the auxiliary agent comprises BYK2070; the particle size of the cesium tungsten bronze slurry is less than or equal to 100nm;
and (2) combining two: the cesium tungsten bronze slurry comprises the following components in parts by weight:
cesium tungsten bronze powder: 10-40 parts of a lubricant; solvent: 50-90 parts; auxiliary agent: 1-10 parts;
wherein, the auxiliary agents comprise BYK2070, BYK7410 and TEGO245; the particle size of the cesium tungsten bronze slurry is less than or equal to 100nm.
In the present invention, in the combination one or the combination two, the weight part of the cesium tungsten bronze powder is preferably 15 to 25 parts, for example, 20 parts.
In the present invention, in the first combination or the second combination, the primary particle diameter of the cesium tungsten bronze powder may be 1 to 20nm, preferably 4 to 20nm.
In the present invention, in the combination one or the combination two, the molecular formula of the cesium tungsten bronze powder can be Cs 0.33 WO 3 。
In the present invention, in the combination one or the combination two, the weight part of the solvent is preferably 50 to 87 parts, for example, 70 parts, 72 parts, 75 parts or 87 parts.
In the present invention, in the combination one, the kind of the solvent is preferably ethanol, toluene or isopropanol.
In the present invention, in the second combination, the solvent may be a solvent capable of dispersing the cesium tungsten bronze powder and the auxiliary agent, which is conventional in the art, preferably ethanol, toluene or isopropanol.
In the present invention, in the combination two, the solvent may not be methyl isobutyl ketone.
In the present invention, the weight part of the auxiliary agent in the combination one or the combination two is preferably 3 to 10 parts, for example 3 parts, 5 parts, 8 parts or 10 parts.
In the present invention, in the combination one or the combination two, the auxiliary agent may further include one or more of BYK161, BYK2025, BYK410, EFKA4310, EFKA4560, EFKA4063, polyethylene glycol 400, polyethylene glycol 600, polypropylene glycol 400, polypropylene glycol 600, polypropylene glycol 2000, TEGO4100, and TEGO 270.
In the second combination, the mass ratio of the BYK2070, the BYK7410 and the TEGO245 in the auxiliary agent can be 2:1:1.
In the present invention, in the combination one or the combination two, the cesium tungsten bronze slurry preferably includes the following components in parts by weight: 10-40 parts of cesium tungsten bronze powder, 50-87 parts of solvent and 3-10 parts of auxiliary agent, for example, 20 parts of cesium tungsten bronze powder, 75 parts of solvent and 5 parts of auxiliary agent, 10 parts of cesium tungsten bronze powder, 87 parts of solvent and 3 parts of auxiliary agent, 20 parts of cesium tungsten bronze powder, 72 parts of solvent and 8 parts of auxiliary agent, or 40 parts of cesium tungsten bronze powder, 50 parts of solvent and 10 parts of auxiliary agent, more preferably comprising the following components in parts by weight: 10-20 parts of cesium tungsten bronze powder, 72-75 parts of solvent and 5-8 parts of auxiliary agent.
In the present invention, in the combination one or the combination two, the particle diameter of the cesium tungsten bronze slurry is preferably 30 to 90nm, more preferably 30 to 60nm, for example 36.39nm, 46.07nm, 51.9nm or 53.14nm.
The invention provides a preparation method of cesium tungsten bronze slurry, which comprises the following steps: and mixing the cesium tungsten bronze powder, the solvent and the auxiliary agent, and performing ball milling treatment to obtain the cesium tungsten bronze slurry.
In the invention, the preparation method of cesium tungsten bronze slurry preferably comprises the following steps: (1) Mixing the cesium tungsten bronze powder, the auxiliary agent and the solvent to obtain dispersion liquid; (2) And ball milling the dispersion liquid to obtain the cesium tungsten bronze slurry.
In the present invention, the mixing process is preferably: firstly, placing the solvent in a reaction kettle, and then adding the cesium tungsten bronze powder and the auxiliary agent.
In the present invention, the mixing process preferably further includes a step of stirring. The stirring time may be 30-50min, for example 40min.
In the present invention, the apparatus for ball milling may be a ball mill.
In the present invention, the rotation speed of the ball milling treatment may be 2000 to 3000rpm, preferably 2500 to 2900rpm, for example 2500rpm, 2600rpm or 2800rpm.
In the present invention, it is preferable to further add grinding balls during the ball milling treatment. The grinding balls may be zirconium beads. The zirconium beads may have a diameter of 0.1 to 0.6mm, for example 0.2mm.
In the present invention, the dispersion liquid is preferably pumped into the ball milling apparatus by a circulation pump during the ball milling process.
In the present invention, the time of the ball milling treatment may be 5 to 9 hours, preferably 6 to 8 hours, for example, 6 hours or 8 hours.
In the present invention, the temperature of the ball milling treatment may be 18 to 40 ℃, preferably 30 to 35 ℃, for example 33 ℃.
The invention also provides application of the cesium tungsten bronze slurry in the field of heat insulation materials.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the invention.
The reagents and materials used in the present invention are commercially available.
The invention has the positive progress effects that:
the invention can prepare cesium tungsten bronze slurry by directly coating cesium tungsten bronze powder in liquid phase without modifying cesium tungsten bronze powder, and the operation method is simple and easy to implement and is easy for industrial production. In the slurry containing cesium tungsten bronze powder, the cesium tungsten bronze powder can be well dispersed in a solvent, and the slurry has the advantages of good infrared heat insulation effect, high light transmittance and the like.
Drawings
FIG. 1 is an external view of cesium tungsten bronze slurry obtained in example 1 after leaving for one week.
Fig. 2 is an external view of cesium tungsten bronze slurry obtained in example 2 after being left for one week.
FIG. 3 is an external view showing the cesium tungsten bronze slurry obtained in example 3 after being left for one week.
Fig. 4 is an external view of cesium tungsten bronze slurry obtained in example 4 after being left for one week.
Fig. 5 is an external view of cesium tungsten bronze slurry obtained in example 5 after being left for one week.
FIG. 6 is an external view showing the cesium tungsten bronze slurry obtained in example 6 after being left for one week.
Fig. 7 is an external view of cesium tungsten bronze slurry obtained in example 7 after being left for one week.
Fig. 8 is an external view of cesium tungsten bronze slurry obtained in example 8 after being left for one week.
Fig. 9 is an external view of cesium tungsten bronze slurry obtained in example 9 after being left for one week.
Fig. 10 is an external view of cesium tungsten bronze slurry obtained in example 10 after being left for one week.
Fig. 11 is an external view of the cesium tungsten bronze slurry obtained in comparative example 1 after being left for one week.
Fig. 12 is an external view of the cesium tungsten bronze slurry obtained in comparative example 2 after being left for one week.
Fig. 13 is an external view of the cesium tungsten bronze slurry obtained in comparative example 3 after being left for one week.
FIG. 14 is a graph showing the particle size distribution of cesium tungsten bronze slurries obtained in examples 1 to 10 and comparative examples 1 to 3.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
The starting materials used in the following examples and comparative examples are all commercially available, wherein cesium tungsten cyanCopper powder Cs 0.33 WO 3 The primary particle size of the catalyst is 4-20nm, the auxiliaries BYK2070 and BYK7410 are purchased from Pick auxiliary company, and the auxiliary TEGO245 is purchased from Digao auxiliary company.
The ball mill used in the preparation of cesium tungsten bronze slurries of the following examples and comparative examples was a sand mill disperser (Pailer sand mill Ashizawa IM 0.5).
Example 1
The cesium tungsten bronze slurry comprises the following components in parts by weight:
cesium tungsten bronze powder Cs 0.33 WO 3 :20 parts; solvent (toluene): 75 parts; auxiliary (BYK 2070): 5 parts.
A method for preparing cesium tungsten bronze slurry, comprising the following steps:
(1) 75 parts of solvent (toluene) is added into a reaction kettle, and 20 parts of cesium tungsten bronze powder Cs are added into the reaction kettle 0.33 WO 3 Adding 5 parts of an auxiliary BYK2070 into a solvent, and uniformly stirring for 40min;
(2) Adding grinding balls into a ball mill, setting the rotating speed at 2800rpm and the ball milling temperature at 33 ℃; and (3) pumping the dispersion liquid in the step (1) to grinding equipment through a circulating pump to grind for 8 hours, and pumping all the dispersion liquid to a reaction kettle to obtain cesium tungsten bronze slurry. Wherein the grinding balls are zirconium beads with the diameter of 0.2mm.
Example 2
The composition of cesium tungsten bronze slurry differs from example 1 only in that: the solvent is methyl isobutyl ketone.
The preparation method of cesium tungsten bronze slurry differs from example 1 only in that: the grinding time in the step (2) is 6h.
Example 3
The composition of cesium tungsten bronze slurry differs from example 2 only in that: the solvent is isopropanol.
Example 4
The composition of cesium tungsten bronze slurry differs from example 2 only in that: ethanol.
Example 5
The composition of cesium tungsten bronze slurry differs from example 4 only in that: the auxiliary agents are BYK2070, BYK7410 and TEGO245, wherein the mass ratio of the BYK2070, the BYK7410 and the TEGO245 is 2:1:1.
The preparation method of cesium tungsten bronze slurry differs from example 4 in that: the ball milling time in the step (2) is 8 hours.
Example 6
The composition of cesium tungsten bronze slurry differs from example 1 in that: 87 parts of solvent and 10 parts of cesium tungsten bronze powder Cs 0.33 WO 3 3 parts of auxiliary agents, wherein the auxiliary agents are BYK2070, BYK7410 and TEGO245, and the mass ratio of the BYK2070, the BYK7410 and the TEGO245 is 2:1:1.
The preparation method of cesium tungsten bronze slurry is different from example 1 in that: in the step (2), the ball milling rotating speed is 2500rpm, and the ball milling time is 6 hours.
Example 7
The composition of cesium tungsten bronze slurry differs from example 1 in that: 50 parts of solvent, 40 parts of cesium tungsten bronze powder Cs 0.33 WO 3 10 parts of auxiliary agents, wherein the auxiliary agents are BYK2070, BYK7410 and TEGO245, and the mass ratio of the BYK2070, the BYK7410 and the TEGO245 is 2:1:1.
The preparation method of cesium tungsten bronze slurry is different from example 1 in that: in the step (2), the ball milling rotating speed is 2600rpm, and the ball milling time is 6 hours.
Example 8
The composition of cesium tungsten bronze slurry differs from example 3 in that: 72 parts of solvent and 8 parts of auxiliary agents, wherein the auxiliary agents are BYK2070, BYK7410 and TEGO245, and the mass ratio of the BYK2070, the BYK7410 and the TEGO245 is 2:1:1.
The preparation method of cesium tungsten bronze slurry is different from example 1 in that: the ball milling time in the step (2) is 7h.
Example 9
The preparation method of cesium tungsten bronze slurry differs from example 5 only in that: the ball milling temperature in the step (2) is 18 ℃.
Example 10
The preparation method of cesium tungsten bronze slurry differs from example 1 only in that: and (3) directly placing cesium tungsten bronze, a solvent and an auxiliary agent in a ball mill for ball milling treatment.
Comparative example 1
The composition of cesium tungsten bronze slurry differs from example 2 only in that: 70 parts of solvent, 30 parts of cesium tungsten bronze powder Cs 0.33 WO 3 。
Comparative example 2
The composition of cesium tungsten bronze slurry differs from example 5 only in that: the solvent is acetone.
The preparation method of cesium tungsten bronze slurry is different from example 1 in that: the rotational speed of the ball milling in the step (2) is 3000rpm, and the ball milling time is 4 hours.
Comparative example 3
The composition of cesium tungsten bronze slurry differs from example 5 in that: 92 parts of solvent, 7 parts of cesium tungsten bronze powder Cs 0.33 WO 3 1 part of an auxiliary agent, wherein the auxiliary agent is BYK2070, BYK7410 and TEGO245, and the mass ratio of the BYK2070, the BYK7410 and the TEGO245 is 2:1:1.
The preparation method of cesium tungsten bronze slurry differs from example 5 in that: the ball milling rotating speed in the step (2) is 1500rpm, and the ball milling time is 10 hours.
Effect examples
The cesium tungsten bronze slurries obtained in examples 1 to 10 and comparative examples 1 to 3 were subjected to stability test, and photographs thereof are shown in fig. 1 to 13, respectively.
The cesium tungsten bronze slurries obtained in examples 1 to 10 and comparative examples 1 to 3 were subjected to particle size testing. The instrument used for the test is a BeNano 90Zeta nanometer particle size and Zeta potential analyzer, the test results are shown in Table 1, and the particle size distribution diagram is shown in FIG. 14.
The cesium tungsten bronze slurries obtained in examples 1 to 10 and comparative examples 1 to 3 were subjected to infrared blocking and light transmittance tests. The instrument used for the test was an LS182 solar film tester, and the test results are shown in Table 1.
TABLE 1
As is clear from the above table, the cesium tungsten bronze slurries prepared in comparative examples 1 to 3 have larger particle diameters (greater than 100 nm) and have poorer infrared blocking rate and visible light transmittance than those of examples 1 to 10.
Claims (10)
1. Cesium tungsten bronze slurry, characterized in that it comprises any one of the following combinations:
combining: the cesium tungsten bronze slurry comprises the following components in parts by weight:
cesium tungsten bronze powder: 10-40 parts of a lubricant; solvent: 50-90 parts; auxiliary agent: 1-10 parts;
wherein the solvent comprises one or more of toluene, methyl isobutyl ketone, isopropanol and ethanol; the auxiliary agent comprises BYK2070; the particle size of the cesium tungsten bronze slurry is less than or equal to 100nm;
and (2) combining two: the cesium tungsten bronze slurry comprises the following components in parts by weight:
cesium tungsten bronze powder: 10-40 parts of a lubricant; solvent: 50-90 parts; auxiliary agent: 1-10 parts;
wherein, the auxiliary agents comprise BYK2070, BYK7410 and TEGO245; the particle size of the cesium tungsten bronze slurry is less than or equal to 100nm.
2. The cesium tungsten bronze slurry according to claim 1, wherein in the combination one or the combination two, the weight fraction of cesium tungsten bronze powder is 15-25 parts, such as 20 parts;
and/or in the first combination or the second combination, the solvent is 50-87 parts by weight, such as 70 parts, 72 parts, 75 parts or 87 parts;
and/or in the first combination or the second combination, the weight part of the auxiliary agent is 3-10 parts, such as 3 parts, 5 parts, 8 parts or 10 parts.
3. The cesium tungsten bronze slurry according to claim 1, wherein in the combination, the kind of the solvent is ethanol, toluene or isopropanol;
and/or, in the second combination, the solvent is ethanol, toluene or isopropanol;
and/or, in the combination two, the solvent is not methyl isobutyl ketone;
and/or, in the first or second combination, the auxiliary agent comprises one or more of BYK161, BYK2025, BYK410, EFKA4310, EFKA4560, EFKA4063, polyethylene glycol 400, polyethylene glycol 600, polypropylene glycol 400, polypropylene glycol 600, polypropylene glycol 2000, TEGO4100, and TEGO 270;
and/or, in the second combination, the mass ratio of the BYK2070, the BYK7410 and the TEGO245 is 2:1:1.
4. The cesium tungsten bronze slurry according to claim 1, wherein in the combination one or the combination two, the cesium tungsten bronze slurry comprises the following components in parts by weight: 10-40 parts of cesium tungsten bronze powder, 50-87 parts of solvent and 3-10 parts of auxiliary agent, for example, 20 parts of cesium tungsten bronze powder, 75 parts of solvent and 5 parts of auxiliary agent, 10 parts of cesium tungsten bronze powder, 87 parts of solvent and 3 parts of auxiliary agent, 20 parts of cesium tungsten bronze powder, 72 parts of solvent and 8 parts of auxiliary agent, or 40 parts of cesium tungsten bronze powder, 50 parts of solvent and 10 parts of auxiliary agent, preferably comprising the following components in parts by weight: 10-20 parts of cesium tungsten bronze powder, 72-75 parts of solvent and 5-8 parts of auxiliary agent.
5. Cesium tungsten bronze slurry according to claim 1, characterized in that in said combination one or said combination two, the particle size of the cesium tungsten bronze slurry is 30-90nm, preferably 30-60nm, such as 36.39nm, 46.07nm, 51.9nm or 53.14nm.
6. A method of preparing cesium tungsten bronze slurry according to any one of claims 1 to 5, characterized in that it comprises the steps of: mixing the cesium tungsten bronze powder, the auxiliary agent and the solvent, and performing ball milling treatment to obtain cesium tungsten bronze slurry;
preferably, the preparation method of the cesium tungsten bronze slurry comprises the following steps: (1) Mixing the cesium tungsten bronze powder, the auxiliary agent and the solvent to obtain dispersion liquid; (2) And ball milling the dispersion liquid to obtain the cesium tungsten bronze slurry.
7. The method of preparing cesium tungsten bronze slurry according to claim 6, wherein the mixing process is: firstly, placing the solvent in a reaction kettle, and then adding the cesium tungsten bronze powder and the auxiliary agent;
and/or, the mixing process further comprises the step of stirring; the stirring time is preferably 30-50min, for example 40min.
8. The method of preparing cesium tungsten bronze slurry according to claim 6, characterized in that the rotational speed of the ball milling treatment is 2000-3000rpm, preferably 2500-2900rpm, such as 2500rpm, 2600rpm or 2800rpm;
and/or the time of the ball milling treatment is 5 to 9 hours, preferably 6 to 8 hours, for example 6 hours or 8 hours;
and/or the temperature of the ball milling treatment is 18-40 ℃, preferably 30-35 ℃, for example 33 ℃.
9. The method for preparing cesium tungsten bronze slurry according to claim 6, wherein grinding balls are further added during the ball milling treatment; the grinding balls are preferably zirconium beads; the zirconium beads preferably have a diameter of 0.1-0.6mm, for example 0.2mm.
10. Use of cesium tungsten bronze slurry according to any one of claims 1 to 5 in the field of insulating materials.
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| CN107513293A (en) * | 2017-08-10 | 2017-12-26 | 广州市黑本新材料科技有限公司 | A kind of preparation method of caesium tungsten bronze modified powder and its slurry |
| CN112552733A (en) * | 2020-12-11 | 2021-03-26 | 三棵树(上海)新材料研究有限公司 | Aqueous cesium tungsten bronze slurry and preparation method thereof |
| CN112961587A (en) * | 2021-02-07 | 2021-06-15 | 三棵树(上海)新材料研究有限公司 | High-stain-resistance glass heat-insulating coating based on cesium tungsten bronze and preparation method thereof |
| CN113681200A (en) * | 2021-09-27 | 2021-11-23 | 烟台佳隆纳米产业有限公司 | Cesium tungsten bronze heat absorbing agent, preparation method thereof and application thereof in transparent ABS infrared welding |
| CN113861601A (en) * | 2021-09-27 | 2021-12-31 | 烟台佳隆纳米产业有限公司 | Cesium tungsten bronze heat absorbing agent, preparation method and application in MS infrared welding |
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| CN107513293A (en) * | 2017-08-10 | 2017-12-26 | 广州市黑本新材料科技有限公司 | A kind of preparation method of caesium tungsten bronze modified powder and its slurry |
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