CN116082826B - Radiation-proof polyurethane elastomer, film and composite glass and preparation method thereof - Google Patents
Radiation-proof polyurethane elastomer, film and composite glass and preparation method thereof Download PDFInfo
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- CN116082826B CN116082826B CN202310127291.XA CN202310127291A CN116082826B CN 116082826 B CN116082826 B CN 116082826B CN 202310127291 A CN202310127291 A CN 202310127291A CN 116082826 B CN116082826 B CN 116082826B
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- 239000011521 glass Substances 0.000 title claims abstract description 48
- 229920003225 polyurethane elastomer Polymers 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000010408 film Substances 0.000 title description 19
- 229920006264 polyurethane film Polymers 0.000 title description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 42
- 229920001971 elastomer Polymers 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 16
- 230000005855 radiation Effects 0.000 claims description 29
- 238000006243 chemical reaction Methods 0.000 claims description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- 239000000806 elastomer Substances 0.000 claims description 16
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 15
- 230000001681 protective effect Effects 0.000 claims description 15
- 150000003077 polyols Chemical class 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 239000004970 Chain extender Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 238000007493 shaping process Methods 0.000 claims description 9
- 239000003054 catalyst Substances 0.000 claims description 8
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 8
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 7
- 125000001931 aliphatic group Chemical group 0.000 claims description 7
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 7
- 238000005266 casting Methods 0.000 claims description 7
- NKTZYSOLHFIEMF-UHFFFAOYSA-N dioxido(dioxo)tungsten;lead(2+) Chemical class [Pb+2].[O-][W]([O-])(=O)=O NKTZYSOLHFIEMF-UHFFFAOYSA-N 0.000 claims description 7
- 229920000570 polyether Polymers 0.000 claims description 7
- 229920005862 polyol Polymers 0.000 claims description 7
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 5
- 229910000464 lead oxide Inorganic materials 0.000 claims description 5
- 229920001451 polypropylene glycol Polymers 0.000 claims description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 4
- 239000004417 polycarbonate Substances 0.000 claims description 4
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 4
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 3
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 3
- 229920000515 polycarbonate Polymers 0.000 claims description 3
- 230000009471 action Effects 0.000 claims description 2
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 abstract description 5
- 238000002156 mixing Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 229910052751 metal Inorganic materials 0.000 description 12
- 239000002184 metal Substances 0.000 description 12
- 239000010410 layer Substances 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229910044991 metal oxide Inorganic materials 0.000 description 6
- 150000004706 metal oxides Chemical class 0.000 description 6
- 239000007822 coupling agent Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000007731 hot pressing Methods 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 2
- 238000005576 amination reaction Methods 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- -1 hydroxylated bismuth tungstate Chemical class 0.000 description 2
- 230000033444 hydroxylation Effects 0.000 description 2
- 238000005805 hydroxylation reaction Methods 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000010907 mechanical stirring Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000012780 transparent material Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000005865 ionizing radiation Effects 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000012994 photoredox catalyst Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- 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
- C08K9/02—Ingredients treated with inorganic substances
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
- B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/40—Layered products comprising a layer of synthetic resin comprising polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
-
- 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
- C08K3/24—Acids; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2475/00—Presence of polyurethane
Abstract
The invention relates to a radiation-proof polyurethane elastomer, a film and composite glass and a preparation method thereof. A radiation-protective polyurethane elastomer comprising: mixing radiation-proof nano particles in the preparation process of the polyurethane elastomer; the content of the radiation-proof nano particles is 5-20wt%. The radiation-proof rubber sheet is prepared from the radiation-proof polyurethane elastomer. The invention solves the problem of reduced mechanical, optical, weather-proof performance and the like caused by directly adding radiation-proof particles into the organic glass.
Description
Technical Field
The application relates to the field of radiation-proof materials, in particular to a radiation-proof polyurethane elastomer, a film, composite glass and a preparation method thereof.
Background
The radiation protective material is capable of absorbing or dissipating radiation energy (commonly referred to as ionizing radiation) in such a way that the radiation is elastically and inelastically scattered by the particles of the substance, such as "compton scattering". The most widely used radiation-proof transparent material is radiation-proof organic glass, which is prepared by reacting methyl methacrylate with metal oxides such as lead, barium, zinc, cadmium and the like to prepare methacrylic acid metal salt, and then polymerizing the methacrylic acid metal salt with methyl methacrylate to prepare the radiation-proof organic glass, wherein the radiation-proof organic glass has certain absorption capacity to X rays, gamma rays and the like. However, the addition of the metal salt can greatly reduce the strength due to the increased brittleness of the organic glass, even lose the function of protecting the structure, and meanwhile, the transmittance, the heat resistance, the solvent resistance and the like are all influenced by the addition amount of the metal salt.
For this purpose, the present invention is proposed.
Disclosure of Invention
The invention mainly aims to provide a radiation-proof polyurethane elastomer, a film, composite glass and a preparation method thereof, which solve the problem of reduced mechanical, optical, weather-proof and other performances caused by directly adding radiation-proof particles into organic glass.
In order to achieve the above object, the present invention provides the following technical solutions.
A first object of the present invention is to provide a radiation-proof polyurethane elastomer comprising:
mixing radiation-proof nano particles in the preparation process of the polyurethane elastomer;
the content of the radiation-proof nano particles is 5-20wt%.
The polyurethane elastomer can be made into films which are widely applied to various organic and inorganic composite transparent pieces, and serve as an intermediate layer to play roles in bonding and buffering and absorbing energy when impacted, nano particles with the radiation protection function are added in the synthesis process of the polyurethane elastomer, so that the radiation protection function can be obtained, and meanwhile, the films can be conveniently compounded with various transparent materials such as organic glass, inorganic glass and polycarbonate in a hot pressing mode, so that the composite transparent piece with the radiation protection function with various structures is obtained. The layers are compounded in a lamination mode, so that the mechanical, optical, weather-proof and other performances of the glass are not adversely affected.
The above radiation protection nanoparticles generally include nanoscale metal oxide particles or nanoscale metal salt particles having a radiation protection function, for example, nanoscale tungsten oxide, nanoscale bismuth oxide, nanoscale lead oxide, nanoscale bismuth tungstate, nanoscale cadmium tungstate, nanoscale barium sulfate, and the like, or modifications thereof.
The content of the radiation protection nano particles can be preferably 5 to 10wt%, 5 to 8wt%, 5 to 7wt% and the like.
On the basis, the types of the nano particles, modification and other factors can influence the mechanical, optical, adhesive, weather resistance and other properties of the material, so that the properties of the elastomer applied to the radiation-proof glass can be optimized in the aspects.
Preferably, the radiation-proof nano particles comprise at least one of a radiation-proof nano metal simple substance, a nano metal oxide, a nano metal salt, a modified nano metal simple substance, a modified nano metal oxide and a modified nano metal salt.
Preferably, the modification in the modified nano metal simple substance, nano metal oxide and modified nano metal salt is as follows: hydroxylation modification, amination modification or coupling agent modification. The surface of the radiation-proof functional nano particles is modified and then added into a polyurethane reaction system, and the functional nano particles are grafted with hydroxyl or amino groups with reactivity so as to increase the compatibility and the binding force of the functional particles and the polyurethane elastomer body. Or grafting functional groups on the surface of the radiation-proof metal oxide/metal salt by using a coupling agent to improve the compatibility with a matrix.
Preferably, the radiation protection nano particles comprise at least one of nano lead, nano bismuth, nano lead oxide, nano bismuth tungstate, nano barium sulfate, hydroxylated lead tungstate nano particles, aminated lead oxide nano particles, KH550 coupled bismuth oxide particles, and titanate coupled barium sulfate particles.
Preferably, the coupling agent comprises at least one of KH570, titanate NDZ-101.
Preferably, the radiation protection nano particles comprise at least one of hydroxylated bismuth tungstate nano particles, hydroxylated cadmium tungstate nano particles, KH570 coupled bismuth powder particles and titanate coupled barium sulfate particles.
These modified nanoparticles all have good compatibility with the polyurethane elastomer body and have strong binding force.
A second aspect of the present invention provides a radiation protective film made from the radiation protective polyurethane elastomer described above.
The elastomer is typically formed into a film using typical shaping techniques such as casting, extrusion, and the like. In addition, the radiation protective nanoparticles may also be incorporated during the shaping of the elastomer into a film. The "radiation-proof polyurethane elastomer" as used herein refers to a broad-sense elastomer, and there is no limitation on the appearance, such as an elastomer in which a film also belongs to a specific shape.
In a third aspect, the invention provides a radiation-proof composite glass, which comprises at least one layer of glass and one layer of radiation-proof film. The glass comprises at least one of inorganic glass, organic glass and polycarbonate.
The lamination of the present invention may be performed by lamination and lamination methods such as bonding and hot pressing.
Preferably, the radiation-proof composite glass comprises inorganic glass, the radiation-proof film, organic glass, the radiation-proof film and organic glass which are stacked in sequence.
The glass compounded by inorganic glass, organic glass and a plurality of layers of radiation-proof films not only has excellent radiation-proof performance, but also reaches excellent level in the aspects of mechanics, optics, weather resistance and the like.
Preferably, each layer in the radiation-proof composite glass is compounded by hot pressing.
A fourth aspect of the present invention provides a process for the preparation of the radiation-protective polyurethane elastomer described above, characterized by comprising:
firstly, performing prepolymerization reaction on aliphatic polyether polyol and aliphatic diisocyanate under the action of a catalyst to obtain NCO-terminated polyurethane elastomer prepolymer;
then, the polyurethane elastomer prepolymer and a polyol chain extender are subjected to chain extension reaction to form an elastomer;
optionally shaping said elastomer to form a radiation-protective polyurethane elastomer of a predetermined shape;
wherein radiation-protective nanoparticles are mixed in at least one of the prepolymerization reaction, the chain extension reaction and the sizing; the addition amount of the radiation-proof nano particles is 5-20wt% of the radiation-proof polyurethane elastomer.
In the prepolymerization reaction, the amount of the aliphatic polyether polyol, the aliphatic diisocyanate, the catalyst and the degree of prepolymerization have important influences on the performance of the elastomer, and the preferable reaction temperature is 75-100 ℃, and the preferable reaction time is 2-4 hours.
Other adjuvants may also be added to the chain extension reaction including, but not limited to, antioxidants, light stabilizers, and the like. The chain extender and prepolymer are generally added in separate cartridges, depending on the properties such as hardness of the elastomer. Vacuum defoaming is also carried out during the reaction, and the temperature is kept at 70-110 ℃.
The above-mentioned optional shaping means that shaping is not required if only the raw material of the particles is required depending on the appearance form of the elastomer. If a specific shape such as a film is required, shaping is required.
Further, the aliphatic polyether polyol comprises one or a mixture of two of polytetrahydrofuran glycol (PTMG) and polyoxypropylene glycol (PPG), and has a molecular weight of 500-3000;
preferably, the aliphatic diisocyanate comprises dicyclohexylmethane diisocyanate (H 12 MDI), hexamethylene Diisocyanate (HDI), isophorone diisocyanate (IPDI);
preferably, the catalyst comprises dibutyltin dilaurate (T-12);
preferably, the catalyst is added in an amount of 0.005 to 0.010wt%;
preferably, the molar ratio of the aliphatic polyether polyol to the aliphatic diisocyanate ranges from (0.2 to 0.4): 1.
further, the polyol chain extender comprises a mixture of one or more of Ethylene Glycol (EG), 1, 4-Butanediol (BDO) and Trimethylolpropane (TMP);
the addition amount of the polyol chain extender enables the hard segment content of the elastomer to be 30-60 wt% and the R value to be in the range of 0.9-1.1.
Further, casting or extrusion means are adopted for shaping.
Preferably, the casting comprises: pouring the material onto a mould, heating to 70-110 ℃, and keeping for 4-8 hours.
Preferably, the temperature of the extrusion is controlled between 90 and 160 ℃.
In conclusion, compared with the prior art, the invention achieves the following technical effects:
(1) In the synthetic process of the transparent polyurethane elastomer, the radiation-proof nano particles are mixed, the mode is simple, the traditional introduction mode of the radiation-proof nano particles is changed, and a new mode is provided for the radiation-proof glass.
(2) The radiation protection function nano particles are modified by hydroxylation, amination, coupling agent and other modes, so that the compatibility and the binding force of the elastomer and the nano particles can be increased.
(3) The preparation conditions of the elastomer are optimized to improve the performances of adhesiveness, light transmittance, mechanics and the like.
(4) The film can be hot-pressed with various transparent parts such as organic glass, inorganic glass, PMMA, PC and the like to obtain the composite transparent part with the radiation protection function in various structural forms.
(5) In the composite glass, compared with inorganic/organic glass, the interlayer is a non-bearing layer, the influence on the performance of the polyurethane interlayer film is small, and the influence on the structural strength of the whole composite transparent piece is small, so that the radiation-proof functional material is a good choice for manufacturing the film.
The foregoing description is only an overview of the technical solutions of the present application, and may be implemented according to the content of the specification in order to make the technical means of the present application more clearly understood, and in order to make the above-mentioned and other objects, features and advantages of the present application more clearly understood, the following detailed description of the present application will be given.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the application. Also, like reference numerals are used to designate like parts throughout the accompanying drawings. In the drawings:
FIG. 1 is a flow chart of the preparation of the radiation-proof polyurethane elastomer provided by the invention.
Detailed Description
Embodiments of the technical solutions of the present application will be described in detail below with reference to the accompanying drawings. The following examples are only for more clearly illustrating the technical solutions of the present application, and thus are only examples, and are not intended to limit the scope of protection of the present application.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having" and any variations thereof in the description and claims of the present application and in the description of the figures above are intended to cover non-exclusive inclusions.
In the description of the embodiments of the present application, the technical terms "first," "second," etc. are used merely to distinguish between different objects and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated, a particular order or a primary or secondary relationship. In the description of the embodiments of the present application, the meaning of "plurality" is two or more unless explicitly defined otherwise.
Reference herein to "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment may be included in at least one embodiment of the present application. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of skill in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments.
In the description of the embodiments of the present application, the term "and/or" is merely an association relationship describing an association object, which means that three relationships may exist, for example, a and/or B may mean: a exists alone, A and B exist together, and B exists alone. In addition, the character "/" herein generally indicates that the front and rear associated objects are an "or" relationship.
In the description of the embodiments of the present application, the term "plurality" refers to two or more (including two), and similarly, "plural sets" refers to two or more (including two), and "plural sheets" refers to two or more (including two).
In the description of the embodiments of the present application, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured" and the like are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally formed; or may be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the embodiments of the present application will be understood by those of ordinary skill in the art according to the specific circumstances.
Example 1
Prepared using the procedure shown in fig. 1:
(1) 150g of lead tungstate nano particles and 200mL of hydrogen peroxide solution are mixed, then ultrasonic oscillation is carried out, the mixture is added into a reaction flask, and the reaction temperature is 120 ℃ and the reaction time is 2 hours by mechanical stirring. And after the reaction is finished, centrifugally separating the mixed solution to obtain hydroxylated lead tungstate nano particles, and washing and drying the hydroxylated lead tungstate nano particles for later use.
(2) Adding 1200g PTMG (molecular weight 2000) into a three-necked flask equipped with a thermometer and a stirrer, vacuum dehydrating at 110deg.C, cooling to below 60deg.C, adding 520g H pre-mixed with 0.1g catalyst 12 MDI is prepolymerized at 85 ℃ for about 4 hours, and the hydroxyl value of the reaction system is sampled and measured at regular intervals until the measured value is basically unchanged, namely the reaction end point.
(3) 120g of hydroxylated lead tungstate nano particles are added into the prepolymer, mechanically stirred for 0.5h at 65 ℃ and added into a material cylinder A of a casting machine, 120g of dehydrated 1,4-BDO chain extender is added into a material cylinder B, uniformly mixed at 85 ℃, and subjected to vacuum defoaming to obtain a reactant.
(4) Injecting the middle material of the casting machine into a glue film mold with the thickness of 2mm, solidifying step by step for 12 hours at 120 ℃, and cooling to obtain the polyurethane film.
(5) A layer of inorganic glass with the thickness of 2.5mm, radiation-proof polyurethane film with the thickness of 2mm, organic glass with the thickness of 10mm, radiation-proof polyurethane film with the thickness of 2mm and organic glass with the thickness of 4mm is subjected to hot pressing at 100 ℃ and 0.8MPa in an autoclave to obtain the composite transparent piece with the radiation-proof function.
Example 2
Unlike the nanoparticles of example 1, which are radiation protective, this example was prepared as follows:
150g of lead oxide nano particles and 100ml of deionized water are added into a flask, ultrasonic treatment is carried out for 20min to prepare a lead oxide aqueous solution, 500ml of ethanol solution is added, 10g of KH550 is added, water bath heating is carried out at 60 ℃, and mechanical stirring reaction is carried out for 10h. And after the reaction is finished, centrifugally separating the mixed solution to obtain aminated lead oxide nano particles, washing with ethanol, and drying for later use.
The remaining steps and amounts of raw materials were the same as in example 1.
Example 3
Unlike the nanoparticles of example 1, which are radiation protective, this example was prepared as follows:
400ml of absolute ethyl alcohol is added into a flask, acetic acid is added to adjust the pH value to 5-6, 150g of bismuth powder is added, and the mixture is placed into an ultrasonic generator for ultrasonic dispersion for 30min. 10g KH570 and 100ml deionized water were added and placed on a magnetic stirrer and stirred for 2h at 80℃in a water bath. After the reaction is finished, centrifugal separation is carried out, absolute ethyl alcohol is used for washing for 3 to 5 times, and KH570 modified bismuth powder particles are obtained through vacuum drying.
The remaining steps and amounts of raw materials were the same as in example 1.
Example 4
Unlike the nanoparticles of example 1, which are radiation protective, this example was prepared as follows:
150g of BaSO4 powder and 500ml of ethanol are added into a flask, dispersed at high speed for 20min, 4g of titanate coupling agent NDZ-101 is added, and the mixture is mechanically stirred and heated in a water bath at 75 ℃ for reflux for 3h. Filtering while the reaction is hot after the reaction is finished, washing the mixture for 3 to 5 times by absolute ethyl alcohol, and drying the mixture in vacuum to obtain NDZ-101 modified BaSO4 particles.
Example 5
The difference from example 1 is only that the amount of radiation protective nanoparticles added is 200g.
Example 6
The only difference from example 1 is that the lead tungstate nanoparticles were not modified and were directly incorporated into the chain extender chain extension reaction.
Example 7
The only difference from example 1 is that "PTMG" was replaced with PPG, having a molecular weight of 2000.
Example 8
The difference from example 1 is only that "H" is 12 MDI "is replaced with HDI.
Example 9
The difference from example 1 is only PTMG and H 12 MDI molar ratios were varied and were 0.4:1.
The results of the elasticity, the mechanical properties, the optical properties, the adhesiveness, and the radiation shielding properties obtained in the step 4 of the above example are shown in Table 1.
The test method of each index is as follows:
the test method is shown in Table 1, wherein the samples of the transmittance, the haze and the X-ray shielding rate are obtained by compounding a layer of polyurethane film with a thickness of 1.2mm and inorganic glass with two sides of 2 mm.
TABLE 1
Note that: "15MeV" for X-ray shielding rate means: [ MEANS FOR SOLVING PROBLEMS ]
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the embodiments, and are intended to be included within the scope of the claims and description. In particular, the technical features mentioned in the respective embodiments may be combined in any manner as long as there is no structural conflict. The present application is not limited to the specific embodiments disclosed herein, but encompasses all technical solutions falling within the scope of the claims.
Claims (12)
1. The preparation method of the radiation-proof polyurethane elastomer is characterized by comprising the following steps:
firstly, performing prepolymerization reaction on aliphatic polyether polyol and aliphatic diisocyanate under the action of a catalyst to obtain NCO-terminated polyurethane elastomer prepolymer;
then, the polyurethane elastomer prepolymer and a polyol chain extender are subjected to chain extension reaction to form an elastomer;
shaping the elastomer to form a radiation-proof polyurethane elastomer with a preset shape;
wherein, radiation-proof nano particles are mixed in the chain extension reaction process; the addition amount of the radiation-proof nano particles is 5-10wt% of the radiation-proof polyurethane elastomer;
the aliphatic polyether polyol comprises one or a mixture of two of polytetrahydrofuran glycol (PTMG) and polypropylene oxide glycol (PPG), and the molecular weight is 500-3000;
the aliphatic diisocyanate comprises one or more of H12MDI, hexamethylene Diisocyanate (HDI) and isophorone diisocyanate (IPDI);
the radiation-proof nano particles comprise at least one of nano lead, nano bismuth, nano lead oxide, nano bismuth tungstate, nano barium sulfate, hydroxylated lead tungstate nano particles, aminated lead oxide nano particles, KH550 coupled bismuth oxide particles and titanate coupled barium sulfate particles; the particle size of the radiation protection nano particles is below 50 nm;
the molar ratio of the aliphatic polyether polyol to the aliphatic diisocyanate ranges from (0.2 to 0.4): 1.
2. the method of preparation of claim 1, wherein the catalyst comprises dibutyltin dilaurate (T-12).
3. The preparation method of claim 1, wherein the catalyst is added in an amount of 0.005-0.010wt%.
4. The method of claim 1, wherein the polyol chain extender comprises a mixture of one or more of Ethylene Glycol (EG), 1, 4-Butanediol (BDO), trimethylolpropane (TMP);
the addition amount of the polyol chain extender enables the hard segment content of the elastomer to be 30-60wt% and the R value to be in the range of 0.9-1.1.
5. The method of claim 1, wherein the shaping is performed by casting or extrusion.
6. The method of manufacturing according to claim 5, wherein the casting comprises: and pouring the material onto a die, heating to 70-110 ℃, and keeping the temperature for 4-8 hours.
7. The method according to claim 5, wherein the extrusion temperature is controlled to be 90-160 ℃.
8. A radiation-protective polyurethane elastomer, characterized in that it is obtainable by the preparation process according to any one of claims 1 to 7.
9. A radiation protective film made from the radiation protective polyurethane elastomer of claim 8.
10. A radiation-proof composite glass, which is characterized by comprising at least one layer of glass and a layer of radiation-proof film according to claim 9; the glass comprises at least one of inorganic glass, organic glass and polycarbonate.
11. The radiation protective composite glass of claim 10, comprising an inorganic glass, the radiation protective film, an organic glass, the radiation protective film, and an organic glass stacked in this order.
12. The radiation protective composite glass of claim 10, wherein the layers in the radiation protective composite glass are hot press compounded.
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