CN116515261A - Cesium tungsten bronze composite PET material and preparation method and application thereof - Google Patents
Cesium tungsten bronze composite PET material and preparation method and application thereof Download PDFInfo
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- CN116515261A CN116515261A CN202310625444.3A CN202310625444A CN116515261A CN 116515261 A CN116515261 A CN 116515261A CN 202310625444 A CN202310625444 A CN 202310625444A CN 116515261 A CN116515261 A CN 116515261A
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- OHUPZDRTZNMIJI-UHFFFAOYSA-N [Cs].[W] Chemical compound [Cs].[W] OHUPZDRTZNMIJI-UHFFFAOYSA-N 0.000 title claims abstract description 82
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910000906 Bronze Inorganic materials 0.000 title claims abstract description 57
- 239000010974 bronze Substances 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 30
- 239000002270 dispersing agent Substances 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 28
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000003960 organic solvent Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 32
- 238000002156 mixing Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical group CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 11
- 238000009413 insulation Methods 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims description 4
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 238000002834 transmittance Methods 0.000 abstract description 9
- 230000004888 barrier function Effects 0.000 abstract description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 51
- 239000005020 polyethylene terephthalate Substances 0.000 description 51
- 230000000052 comparative effect Effects 0.000 description 9
- 238000001125 extrusion Methods 0.000 description 7
- 230000000903 blocking effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000002086 nanomaterial Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 239000011147 inorganic material Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000005469 granulation Methods 0.000 description 2
- 230000003179 granulation Effects 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000010438 heat treatment Methods 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
- QPJVMBTYPHYUOC-UHFFFAOYSA-N methyl benzoate Chemical group COC(=O)C1=CC=CC=C1 QPJVMBTYPHYUOC-UHFFFAOYSA-N 0.000 description 2
- 238000003801 milling Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920000620 organic polymer Polymers 0.000 description 2
- 235000011837 pasties Nutrition 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- -1 polyethylene terephthalate Polymers 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 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
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000005344 low-emissivity glass Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229940095102 methyl benzoate Drugs 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004753 textile 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/2053—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the additives only being premixed with a liquid phase
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2475/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2475/04—Polyurethanes
-
- 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
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- 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
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a cesium tungsten bronze composite PET material and a preparation method and application thereof. The cesium tungsten bronze composite PET material comprises, by total weight 100 parts, 85-95 parts of PET master batch and 5-15 parts of CWO dispersion liquid; wherein the CWO dispersion comprises the following components: 20-50 parts of cesium tungsten bronze powder; the organic solvent is less than or equal to 70 parts; 10-40 parts of dispersing agent; in the CWO dispersion, cesium tungsten bronze powder has a size of 10-100nm. The cesium tungsten bronze composite PET material has excellent infrared barrier property and higher visible light transmittance, and the preparation method is simple.
Description
Technical Field
The invention particularly relates to a cesium tungsten bronze composite PET material, and a preparation method and application thereof.
Background
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 energy consumption of the building is in a trend of increasing year by year at present. Therefore, the development of novel heat insulation materials has become a great trend of energy conservation 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, which shows reflection of solar heat, and generally requires a complex coating structure and a plurality of functional layers, and has high requirements on the process and equipment, so that the application cost is high. 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.
Cesium tungsten bronze (CWO) is a nano-scale inorganic material capable of absorbing near infrared light having a wavelength of 900 to 2000 nanometers. The heat-insulating and infrared-proof product prepared from cesium tungsten bronze powder can greatly improve the comfort of a human body, greatly save energy and realize more effective warmth in winter and coolness in summer. However, cesium tungsten bronze nano-materials have higher surface activity and adsorptivity and are easy to agglomerate.
The polyethylene terephthalate (PET) has rigid groups on the molecular main chain and high symmetry of the molecular chain, so that the polyethylene terephthalate has excellent physical and mechanical properties, heat resistance, electrical properties and film forming property, and is low in cost. Accordingly, PET is widely used in engineering plastics, fiber textiles and film industry. Currently, the main method for improving the infrared barrier property of PET materials is to add a certain amount of inorganic materials with infrared heat insulation absorption. However, when the added inorganic material is compounded with the organic polymer, the problems of dispersibility and compatibility among substances exist, so that the light transmittance of the infrared barrier film is reduced; particularly, when the cesium tungsten bronze nanomaterial is used in combination with resin, the resin is difficult to disperse due to the generally high viscosity, so that the infrared ray absorption performance of the cesium tungsten bronze nanomaterial can be greatly reduced.
Disclosure of Invention
The invention solves the technical problem of overcoming the defect of poor infrared barrier property in the prior art when cesium tungsten bronze nano-materials are matched with resin for use, and provides a cesium tungsten bronze composite PET material and a preparation method and application thereof. The cesium tungsten bronze composite PET material has excellent infrared barrier property and higher visible light transmittance, and the preparation method is simple.
In the prior art, PET and cesium tungsten bronze powder are composited and used as described in chinese patent document CN110713701a, but the patent has drawbacks of uneven dispersion, large particle size, low visible light transmittance and high haze value in the process of compositely using the two. In the application, the inventor creatively finds that the infrared blocking performance and the visible light transmittance of the cesium tungsten bronze composite PET material can be effectively improved by adopting a specific amount of dispersing agent to be matched with PET master batch and cesium tungsten bronze powder for use and adjusting the amount of each component and the particle size of the cesium tungsten bronze powder in dispersion liquid; further, the inventor can make the performance of the cesium tungsten bronze composite PET material more optimized by adding a specific kind of organic solvent into the system.
The invention solves the technical problems by the following technical proposal:
the invention provides a cesium tungsten bronze composite PET material, which comprises, by total weight 100 parts, 85-95 parts of PET master batch and 5-15 parts of CWO dispersion liquid;
wherein the CWO dispersion comprises the following components:
20-50 parts of cesium tungsten bronze powder;
the organic solvent is less than or equal to 70 parts;
10-40 parts of dispersing agent;
in the CWO dispersion liquid, the size of the cesium tungsten bronze powder is 10-100nm.
In the present invention, the PET master batch can be obtained by conventional commercial use.
In the present invention, the PET master batch is preferably used in an amount of 88 to 92 parts, for example, 90 parts.
In the present invention, the CWO dispersion is preferably used in an amount of 8 to 12 parts, for example, 10 parts.
In the CWO dispersion of the present invention, the size of the cesium tungsten bronze powder is preferably 20 to 60nm, more preferably 30 to 50nm, for example 40nm, 42nm or 43nm.
In the preparation process of the CWO dispersion liquid, the organic solvent volatilizes to a certain extent.
In the present invention, preferably, the CWO dispersion comprises the following raw material components:
20-50 parts of cesium tungsten bronze powder;
20-70 parts of an organic solvent;
10-40 parts of dispersing agent.
Wherein the amount of the organic solvent is preferably 25 to 45 parts, for example 30 parts or 40 parts.
In the present invention, the boiling point of the organic solvent is preferably lower than 100 ℃.
In the present invention, the organic solvent is preferably one or more of an alcohol solvent, a ketone solvent and an ester solvent.
Wherein the alcoholic solvent is preferably ethanol and/or isopropanol, such as isopropanol.
Wherein the ketone solvent is preferably acetone and/or butanone, such as acetone.
Wherein the ester solvent is preferably ethyl acetate.
In the invention, the dispersing agent generally refers to a substance which can provide the same charge, leads the surface of the powder to have the same charge to generate repulsion, and has the secondary branched chain of a high polymer long chain, and can provide certain steric hindrance to increase the space between the powder bodies, thereby reducing the aggregation of solid or liquid particles in a dispersing system through the same charge repulsion and steric hindrance.
In the present invention, the dispersant is preferably a polyurethane-based dispersant.
The polyurethane dispersant is preferably EFKA4560 and/or EFKA4063.
In the present invention, the dispersant is preferably used in an amount of 25 to 35 parts, for example, 30 parts.
In the present invention, the cesium tungsten bronze powder can be obtained by conventional commercial use.
In the present invention, the cesium tungsten bronze powder is preferably used in an amount of 25 to 45 parts, for example, 30 parts or 40 parts.
In a preferred embodiment, the cesium tungsten bronze composite PET material comprises 90 parts of PET master batch, 4 parts of cesium tungsten bronze powder, 3 parts of isopropanol and 3 parts of EFKA4063 dispersing agent.
In a preferred embodiment, the cesium tungsten bronze composite PET material comprises 90 parts of PET master batch, 4 parts of cesium tungsten bronze powder, 3 parts of ethyl acetate and 3 parts of EFKA4063 dispersing agent.
In a preferred embodiment, the cesium tungsten bronze composite PET material comprises 90 parts of PET master batch, 4 parts of cesium tungsten bronze powder, 3 parts of acetone and 3 parts of EFKA4063 dispersing agent.
In a preferred embodiment, the cesium tungsten bronze composite PET material comprises 90 parts of PET master batch, 3 parts of cesium tungsten bronze powder, 4 parts of isopropanol and 3 parts of EFKA4063 dispersing agent.
The invention also provides a preparation method of the cesium tungsten bronze composite PET material, which comprises the following steps:
and mixing the CWO dispersion liquid subjected to ball milling treatment for 5-10 hours with the PET master batch to obtain the PET master batch.
In the invention, the cesium tungsten bronze composite PET material can be pasty.
In the invention, the preparation method of the CWO dispersion liquid can be conventional in the art, and raw materials are generally mixed and ball-milled.
Wherein the mixing equipment may be conventional in the art, such as a high speed disperser.
Wherein the rotational speed of the mixing is preferably 1000-2000rpm, e.g. 1400rpm.
Wherein the mixing time is preferably 30-90min, for example 60min.
In the present invention, the apparatus for the ball milling treatment may be conventional in the art, such as a mill disperser.
In the present invention, the rotation speed of the ball milling treatment may be 2500 to 3500rpm, for example, 3000rpm.
In the present invention, the time of the ball milling treatment is preferably 6 to 9 hours, for example 8 hours.
In the ball milling process, the milling balls may be conventional in the art, such as zirconium beads.
In the ball milling treatment, the diameter of the milling balls may be 0.1 to 0.6mm, for example, 0.1mm.
In the present invention, the mixing apparatus may be conventional in the art, such as a blender.
In the present invention, the mixing means may be conventional in the art, such as stirring.
In the present invention, the stirring speed during the mixing is preferably 500 to 1000rpm, for example 800rpm.
In the present invention, the stirring time during the mixing is preferably 5 to 30 minutes, for example, 10 minutes.
In the invention, the cesium tungsten bronze composite PET material can be obtained after the mixing. The cesium tungsten bronze composite PET material may be pasty.
In the present invention, the mixing is preferably further followed by melt extrusion and granulation. After granulation, the granular cesium tungsten bronze composite PET material can be generally obtained.
The apparatus for melt extrusion and pelletization may be conventional in the art, such as a twin screw extruder. The aspect ratio of the twin screw extruder may be conventional in the art, for example 30:1.
wherein the temperature of the melt extrusion is preferably 270 ℃ to 280 ℃, for example 275 ℃.
Wherein, during the melt extrusion, the screw speed is preferably 100-150rpm, for example 120rpm.
In a preferred embodiment, the melt extrusion and pelletization employ an aspect ratio of 30:1, the processing temperature is 275 ℃, the melting plasticization is carried out under the condition of the screw rotating speed of 120rpm, and the cesium tungsten bronze composite PET material is prepared through a T-shaped die with an opening of 0.6 mm.
The invention also provides application of the cesium tungsten bronze composite PET material in heat insulation and infrared prevention products.
In the invention, the heat-insulating and infrared-proof product can be any product, such as a film, a plate or heating and heat-preserving fiber.
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:
(1) The cesium tungsten bronze composite PET material has excellent infrared blocking performance and higher visible light transmittance;
(2) In the cesium tungsten bronze composite PET material, the cesium tungsten bronze nano material can be uniformly distributed, so that the problem of agglomeration of cesium tungsten bronze nano particles is effectively solved;
(3) The cesium tungsten bronze composite PET material has excellent mechanical properties;
(4) The preparation method of the cesium tungsten bronze composite PET material is simple, can be used for industrial production, and is directly used for producing high-transparency high-heat-insulation films, plates, heating thermal-insulation fibers and the like.
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 information on the raw materials used in the following examples and comparative examples is shown in table 1 below:
TABLE 1
The model manufacturers of the equipment used in the following examples and comparative examples are shown in Table 2 below:
TABLE 2
| Device name | Model number | Manufacturer' s |
| Grinding and dispersing machine | Ashizawa IM | Pailer (Pailer) |
| High-speed dispersing machine | TGM-FL | General intelligent |
| Double screw extruder | RXT | CPM extrusion group |
| Solar film tester | LS182 | Technology on forests |
| Table type integrating sphere spectrophotometer | Ci7 | Aishenli (Chinese character) |
Example 1
(1) Preparing nano CWO nano dispersion liquid:
30 parts of isopropanol (organic solvent), 30 parts of EFKA4063 (dispersing agent) and 40 parts of nano CWO powder are respectively taken in a reaction kettle, are pre-mixed for 60min by adopting a high-speed dispersing machine at 1400rpm, and are then sanded for 8 hours by adopting 0.1mm zirconium beads on a grinding dispersing machine at a rotating speed of 3000rpm, so as to prepare a CWO dispersion.
(2) 90 parts of PET master batch and 10 parts of CWO dispersion are put into a stirrer, and stirred at a high speed for 10 minutes at a rotation speed of 800rpm to be uniformly mixed, thus obtaining the cesium tungsten bronze composite PET material.
The cesium tungsten bronze composite PET material described above was then dosed into the aspect ratio 30:1, the processing temperature is set at 275 ℃, the melting plasticization is carried out under the condition of the screw rotating speed of 120rpm, the cesium tungsten bronze composite PET master batch with uniform diameter is formed by a T-shaped die with an opening of 0.6mm, and the cesium tungsten bronze composite PET master batch is cooled and sheared into uniform granular cesium tungsten bronze composite PET master batch.
Example 2
The procedure and conditions were the same as in example 1, except that isopropyl alcohol in step (1) was replaced with ethyl acetate.
Example 3
The procedure and conditions were the same as in example 1, except that isopropanol in step (1) was replaced with acetone.
Example 4
The feeding proportion in the step (1) is 40 parts of isopropanol, 30 parts of EFKA4063 and 30 parts of nano CWO powder;
the procedure and conditions were the same as in example 1, except that the amounts of the components added in step (1) were different.
Comparative example 1
The procedure and conditions were the same as in example 1, except that the dispersant EFKA4063 in step (1) was replaced with the modified acrylate dispersant BYK 2055.
Comparative example 2
The procedure and conditions were the same as in example 1, except that isopropyl alcohol in step (1) was replaced with methyl benzoate.
Comparative example 3
The feeding proportion in the step (1) is 30 parts of isopropanol, 5 parts of EFKA4063 and 40 parts of nano CWO powder;
the procedure and conditions were the same as in example 1, except that the amounts of the components added in step (1) were different.
Comparative example 4
Respectively taking 3 parts of isopropanol, 3 parts of EFKA4063, 4 parts of nano CWO powder and 90 parts of PET master batch, putting into a stirrer, and stirring at a high speed for 10 minutes at a speed of 800rpm to uniformly mix. The above mixture is then dosed into the aspect ratio 30:1, the processing temperature is set at 275 ℃, the melting plasticization is carried out under the condition of the screw rotating speed of 120rpm, the infrared blocking PET composite functional master batch with uniform diameter is formed through a T-shaped die with an opening of 0.6mm, and the infrared blocking PET composite functional master batch is cooled and sheared into uniform granular master batch.
Comparative example 5
The operation and conditions were the same as in example 1 except that the ball milling time in step (1) was adjusted to 12 hours.
Effect examples
The infrared barrier and transmittance of the samples were measured using an LS182 solar film tester.
The haze of the samples was measured using a bench-top integrating sphere spectrophotometer.
Performance tests were performed on cesium tungsten bronze composite PET master batches prepared in examples 1-4 and comparative examples 1-5, as shown in the following table 3 data:
TABLE 3 Table 3
According to the embodiment 1-4, the nano CWO dispersion liquid added with the dispersing agent can be uniformly dispersed and better fused with the organic polymer in the process of preparing the cesium tungsten bronze composite PET master batch by melt blending extrusion, so that the cesium tungsten bronze composite PET master batch is endowed with higher infrared blocking rate and visible light transmittance; from comparative examples 1 to 5, it can be seen that when other types of dispersants or organic solvents are used, or technological parameters are adjusted (raw material mixing mode is changed or ball milling time is changed), the prepared cesium tungsten bronze composite PET master batch has larger particle size, poor dispersing effect, increased haze and poor external blocking and transparency of the prepared product.
Claims (10)
1. The cesium tungsten bronze composite PET material is characterized by comprising, by total weight of 100 parts, 85-95 parts of PET master batch and 5-15 parts of CWO dispersion;
wherein the CWO dispersion comprises the following components:
20-50 parts of cesium tungsten bronze powder;
the organic solvent is less than or equal to 70 parts;
10-40 parts of dispersing agent;
in the CWO dispersion liquid, the size of the cesium tungsten bronze powder is 10-100nm.
2. The cesium tungsten bronze composite PET material of claim 1, wherein the cesium tungsten bronze composite PET material meets one or more of the following conditions:
(1) The PET master batch is used in an amount of 88-92 parts, for example 90 parts;
(2) The CWO dispersion is used in an amount of 8-12 parts, for example 10 parts;
(3) The dispersant is used in an amount of 25 to 35 parts, for example 30 parts;
(4) The cesium tungsten bronze powder is used in an amount of 25-45 parts, for example 30 parts or 40 parts; and
(5) In the CWO dispersion, the cesium tungsten bronze powder has a size of 20 to 60nm, preferably 30 to 50nm, for example 40nm, 42nm or 43nm.
3. The cesium tungsten bronze composite PET material of claim 1, wherein the organic solvent is one or more of an alcohol solvent, a ketone solvent, and an ester solvent;
the alcoholic solvent is preferably ethanol and/or isopropanol, such as isopropanol;
the ketone solvent is preferably acetone and/or butanone, for example acetone;
the ester solvent is preferably ethyl acetate.
4. The cesium tungsten bronze composite PET material of claim 1, wherein the CWO dispersion comprises the following raw material components:
20-50 parts of cesium tungsten bronze powder;
20-70 parts of an organic solvent;
10-40 parts of dispersing agent;
wherein the organic solvent is preferably used in an amount of 25 to 45 parts, for example 30 parts or 40 parts;
and/or the dispersing agent is polyurethane dispersing agent;
the polyurethane dispersant is preferably EFKA4560 and/or EFKA4063.
5. The cesium tungsten bronze composite PET material according to claim 1, wherein the raw materials of the cesium tungsten bronze composite PET material comprise 90 parts of PET master batch, 4 parts of cesium tungsten bronze powder, 3 parts of isopropanol and 3 parts of EFKA4063 dispersant;
or, the cesium tungsten bronze composite PET material comprises 90 parts of PET master batch, 4 parts of cesium tungsten bronze powder, 3 parts of ethyl acetate and 3 parts of EFKA4063 dispersing agent;
or, the cesium tungsten bronze composite PET material comprises 90 parts of PET master batch, 4 parts of cesium tungsten bronze powder, 3 parts of acetone and 3 parts of EFKA4063 dispersing agent;
or, the cesium tungsten bronze composite PET material comprises 90 parts of PET master batch, 3 parts of cesium tungsten bronze powder, 4 parts of isopropanol and 3 parts of EFKA4063 dispersing agent.
6. A method for preparing the cesium tungsten bronze composite PET material according to any one of claims 1 to 5, characterized in that it comprises the following steps:
and mixing the CWO dispersion liquid subjected to ball milling treatment for 5-10 hours with the PET master batch to obtain the PET master batch.
7. The method for preparing the cesium tungsten bronze composite PET material according to claim 6, wherein the preparation method of the CWO dispersion liquid is to mix raw materials and ball mill;
in the preparation of the CWO dispersion, the mixing speed is preferably 1000 to 2000rpm, for example 1400rpm;
in the preparation of the CWO dispersion, the mixing time is preferably 30 to 90 minutes, for example 60 minutes.
8. The method for preparing cesium tungsten bronze composite PET material according to claim 6, characterized in that the rotation speed of the ball milling treatment is 2500-3500rpm, for example 3000rpm;
and/or the ball milling treatment is carried out for a period of time ranging from 6 to 9 hours, for example 8 hours.
9. The method of preparing cesium tungsten bronze composite PET material according to claim 6, wherein during the mixing, the rotational speed of stirring is 500-1000rpm, such as 800rpm;
and/or, during said mixing, the stirring time is between 5 and 30 minutes, for example 10 minutes.
10. Use of the cesium tungsten bronze composite PET material of any one of claims 1 to 5 in heat insulation and infrared protection products.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310625444.3A CN116515261A (en) | 2023-05-30 | 2023-05-30 | Cesium tungsten bronze composite PET material and preparation method and application thereof |
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| CN202310625444.3A CN116515261A (en) | 2023-05-30 | 2023-05-30 | Cesium tungsten bronze composite PET material and preparation method and application thereof |
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