TR201411519A2 - Improvements in surface properties of the glass beads which are used as retrorefrective material in road markings by coating with natural clay - Google Patents
Improvements in surface properties of the glass beads which are used as retrorefrective material in road markings by coating with natural clay Download PDFInfo
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- TR201411519A2 TR201411519A2 TR2014/11519A TR201411519A TR201411519A2 TR 201411519 A2 TR201411519 A2 TR 201411519A2 TR 2014/11519 A TR2014/11519 A TR 2014/11519A TR 201411519 A TR201411519 A TR 201411519A TR 201411519 A2 TR201411519 A2 TR 201411519A2
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- Prior art keywords
- glass
- paint
- glass beads
- feature
- montmorillonite
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- 239000011521 glass Substances 0.000 title claims abstract description 77
- 239000011324 bead Substances 0.000 title claims abstract description 42
- 238000000576 coating method Methods 0.000 title claims description 24
- 239000011248 coating agent Substances 0.000 title claims description 21
- 239000000463 material Substances 0.000 title claims description 16
- 239000004927 clay Substances 0.000 title claims description 11
- 239000003973 paint Substances 0.000 claims abstract description 77
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910052901 montmorillonite Inorganic materials 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- QXJJQWWVWRCVQT-UHFFFAOYSA-K calcium;sodium;phosphate Chemical compound [Na+].[Ca+2].[O-]P([O-])([O-])=O QXJJQWWVWRCVQT-UHFFFAOYSA-K 0.000 claims description 33
- 239000000725 suspension Substances 0.000 claims description 16
- 238000005341 cation exchange Methods 0.000 claims description 10
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 8
- 239000011230 binding agent Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007900 aqueous suspension Substances 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 229930014626 natural product Natural products 0.000 claims description 2
- 238000007654 immersion Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract description 7
- 229910000077 silane Inorganic materials 0.000 abstract description 7
- 230000007423 decrease Effects 0.000 description 7
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 230000002209 hydrophobic effect Effects 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229920002689 polyvinyl acetate Polymers 0.000 description 3
- 229940075065 polyvinyl acetate Drugs 0.000 description 3
- 239000011118 polyvinyl acetate Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 150000004756 silanes Chemical class 0.000 description 3
- 239000004484 Briquette Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 239000013065 commercial product Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 238000011206 morphological examination Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
- C03C12/02—Reflective beads
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1055—Coating or impregnating with inorganic materials
- C04B20/1074—Silicates, e.g. glass
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
-
- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01F—ADDITIONAL WORK, SUCH AS EQUIPPING ROADS OR THE CONSTRUCTION OF PLATFORMS, HELICOPTER LANDING STAGES, SIGNS, SNOW FENCES, OR THE LIKE
- E01F9/00—Arrangement of road signs or traffic signals; Arrangements for enforcing caution
- E01F9/50—Road surface markings; Kerbs or road edgings, specially adapted for alerting road users
- E01F9/506—Road surface markings; Kerbs or road edgings, specially adapted for alerting road users characterised by the road surface marking material, e.g. comprising additives for improving friction or reflectivity; Methods of forming, installing or applying markings in, on or to road surfaces
- E01F9/524—Reflecting elements specially adapted for incorporation in or application to road surface markings
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/12—Reflex reflectors
- G02B5/126—Reflex reflectors including curved refracting surface
- G02B5/128—Reflex reflectors including curved refracting surface transparent spheres being embedded in matrix
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/228—Other specific oxides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/0075—Uses not provided for elsewhere in C04B2111/00 for road construction
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/60—Flooring materials
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Architecture (AREA)
- Civil Engineering (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Road Signs Or Road Markings (AREA)
- Paints Or Removers (AREA)
- Road Paving Structures (AREA)
- Road Repair (AREA)
- Surface Treatment Of Glass (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Optical Elements Other Than Lenses (AREA)
Abstract
Description
TARIFNAMEW Bulusun Ilqili Oldugu Teknik Saha Bulus, uygulamasi özellikle çevre dostu su bazli yol çizgi boyalarinda gerçeklestirilmis olup, yoI çizgi boyalarinda gece görünürlülügünü arttiran cam kürecik yüzeylerinin daldirma yöntemiyle nanoboyutlu inorganik esasli dogal bir kil (montmorillonit) ve/veya modifiye kil ile kaplanmasi, kaplama sonucunda da cam küre yüzey özelliklerinin gelistirilerek, ticari benzerlerine göre yüksek retroreflektif özellige sahip, asinma direnci daha yüksek dolayisiyla uzun ömürlü gece görünürlügüne sahip boya uygulamasina olanak saglayan, ucuz cam küreciklerin elde edilmesi ile ilgilidir. DESCRIPTION Technical Field to which the Invention Relates The application of the invention is especially in environmentally friendly water-based road marking paints. glass that increases night visibility in road marking paints. A nano-sized inorganic-based natural clay with the dipping method of the spherical surfaces. (montmorillonite) and/or modified clay, resulting in glass By improving the spherical surface properties, it is highly retroreflective compared to its commercial counterparts. feature, with higher abrasion resistance, therefore, long-lasting night Inexpensive glass beads that allow the application of paint with high visibility. it's about getting it.
Teknigin Bilinen Durumu Cam küreler boya uygulamasinin hemen ardindan farkli gradasyonda olacak sekilde boya yüzeyine yayilmakta olup en büyük boyutlular en üstte, düsük boyutlular alta yerlesecek sekilde uygulama gerçeklestirilmektedir. Bu uygulamanin uygun olmasi gece görünürlügü açisindan çok önemli olan retroreflektif özellikte yol çizgi boyalari elde edilmesinde kritik bir öneme sahiptir [1,2,3]. Cam küre parçaciklari serbest akis göstermez ise istenilen düzgün dagilim saglanamamaktadir. Tane boyutu küçük kürelere cam yüzeyinde bulunan hidrofilik -OH grubu nedeniyle nem etki etmekte ve topaklanma problemi ortaya çikabilmektedir. Topaklanma, cam küre yüzeyinin hidrofobik kaplanmasi ile önlenebilmektedir. Ancak, cam küre yüzeyindeki hidrofobik kaplama malzemesi ile boya arasinda iyi bir adhezyon saglanmamasi durumunda trafik altinda cam kürecikler boya yüzeyinden kolayca kopabilmektedir. Dolayisi ile retroreflektif kaybina neden olan uygulamalar söz konusu olabilmektedir. Bunu önlemek için de arada ayrica baglayici ajan kullanimi gerçeklestirilmektedir. Ancak bu durumda da boya cam küre yüzeyini çok kaplamakta ve sonuçta retroreflektivite düsmektedir. Ayrica, baglayici ajanlar hidrofobik olmadigi için topaklanma probleminin artisina da neden olabilmektedir [2]. State of the Art Glass spheres should be in different gradation immediately after paint application. spreads over the paint surface and the largest sizes are at the top, the lower ones are at the bottom. The application is carried out in such a way that it is settled. The suitability of this application Road marking paints with retroreflective properties, which are very important in terms of night visibility. It has a critical importance in obtaining it [1,2,3]. Glass sphere particles free flowing If it does not show the desired smooth distribution cannot be achieved. Small grain size Spheres are affected by moisture due to the hydrophilic -OH group on the glass surface and agglomeration problem may occur. Clumping of the glass ball surface can be prevented by its hydrophobic coating. However, the hydrophobic If good adhesion is not provided between the coating material and the paint. Glass beads can easily break from the paint surface under traffic. Due to There may be applications that cause retroreflective loss. this much In order to prevent this, a binding agent is also used in between. However In this case, too, the paint covers the surface of the glass ball too much, resulting in retroreflectivity. is falling. In addition, because the binding agents are not hydrophobic, agglomeration It can also cause an increase in the problem [2].
Baslangiçta büyük boyutlu cam kürelerin yüzeyde olmasina bagli olarak yüksek olan retroreflektivite zamanla araçlarin üzerinden geçmesi yani mekanik etkiler ve boyanin asinmasiyla birlikte retroreflektivite degeri paralel olarak azalis göstermektedir. Cam küre asinmasi sonucu olusan bosluklar tozla kaplanip yüzey grilesmekte ve hem gece hem de gündüz retroreflektivitesi azalmaktadir. Initially high due to the large sized glass spheres on the surface. retroreflectivity, that is, passing over vehicles over time, that is, mechanical effects and paint With wear, the retroreflectivity value decreases in parallel. Pine The cavities formed as a result of the wear of the sphere are covered with dust and the surface becomes gray and both both night and day retroreflectivity decreases.
Yüzey modifikasyonu yapilmamis olan cam kürelerin boya ile adezyonu düsük olacagindan, boya içerisindeki cam kürelerin kopmasi daha kolaydir. Glass spheres without surface modification have low adhesion with paint. It will be easier for the glass spheres in the paint to break off.
Literatüidgmgm üstesinden gelebilmek için cam kürecikler polimerik yama organik esasli çesitli malzemelerle kaplanmistir. kürenin kaplanmasinda kullanilmistir [4]. US3222204 nolu patentde florokarbonlar kullanilmistir. Her iki uygulama da pahalidir ve olusan ürünlerin performans testleri sonrasi yipranmasi fazladir. Yani yol çizgi boyasi üzerinden tasit geçtikçe cam kürelerin boya yüzeyinden kopmasi fazladir [5]. elde edilen poliüretan esasli polimerik malzemelerle cam kürecikler kaplanmistir. Bu yöntem de pratik olmayan pahali bir yöntemdir ve istenilen performans sonuçlara ulasilamamaktadir [1]. Glass beads polymeric patch to overcome literature idgmgm It is coated with various organic-based materials. It was used in the coating of the sphere [4]. Fluorocarbons in patent US3222204 used. Both applications are expensive and the performance tests of the resulting products wear is excessive. That is, as the vehicle passes over the road marking paint, the glass the rupture of the spheres from the paint surface is high [5]. Glass beads were coated with the obtained polyurethane-based polymeric materials. This method is also an impractical and expensive method and the desired performance results in results. cannot be reached [1].
Literatürde çogunlukla hidrofobik yapisi nedeniyle silan bilesikleri kaplama malzemesi olarak kullanilmistir. Ticari uygulamalarda da silan bilesikleri ile kapli cam bu uygulamalar kapsiz cam kürelere ve diger uygulamalara kiyasla daha pratik olmakla birlikte bu çalismadan da görülebilecegi gibi daha çevreci, daha ucuz ve dogal malzemeler bulunabilir [6,7,8,9]. kullanilmistir [3]. peroksit ile karistirilmistir. Bu çalisma daha karmasik, özel bir dikkat gerektirdigi için pahali bir kaplama yöntemidir [10,11] Ayrica benzoil peroksit uçucu ve alev alici bir malzeme oldugundan süreç içerisinde kaplama etkisi azalacak alev alma tehlikesi de söz konusu olabilecektir. In the literature, silane compounds are mostly used for coating due to their hydrophobic nature. was used as the material. Glass coated with silane compounds also in commercial applications these applications are more practical compared to uncapped glass balls and other applications However, as can be seen from this study, it is more environmentally friendly, cheaper and natural materials can be found [6,7,8,9]. has been used [3]. mixed with peroxide. This study is more complex, as it requires special attention. It is an expensive coating method [10,11] In addition, benzoyl peroxide is a volatile and flammable Since it is a material, the coating effect will decrease in the process and the danger of flaming is also present. may occur.
WOO1/42349 patentinde digerlerinden farkli olarak cam küreler poli vinil asetat ile kaplanmistir. Kaplanan cam küreler yol çizgi boyasina serpildikten sonra bir yil içerisindeki gece görünürlülügü degerleri ölçülmüstür. Sonuçlara göre polivinil asetat kaplamali cam kürelerin boyaya tutunmasinin kaplamasiz cam kürelere göre daha iyi oldugu görülmektedir. Ancak silan kapli ticari ürünler ile herhangi bir karsilastirma yapilmamistir. Ayrica polivinil asetat, silan bilesiklerine göre daha pahali olabilmektedir [10]. In the WOO1/42349 patent, unlike the others, the glass spheres are made of poly vinyl acetate. is covered. One year after the coated glass balls are sprinkled on the road marking paint Night visibility values in the interior were measured. According to the results polyvinyl acetate Coated glass balls have better adhesion to paint than uncoated glass balls. appears to be. However, any comparison with silane-coated commercial products not done. In addition, polyvinyl acetate is more expensive than silane compounds. can be [10].
Söz konusu bulus ile ticari ürünler ile rekabet edebilecek, inorganik esasli, ucuz, uygulamasi kolay ve çevreye zarari olmayan ve özellikle çevre dostu su bazli yol çizgi boyasi ile oldukça uyumlu asinma direnci yüksek &yüksek retroreflektif . özellige &p cam kürecikler elde edilebilmektedir. With the said invention, inorganic based, cheap, easy to apply and environmentally friendly, especially environmentally friendly water-based road Highly abrasion resistant & highly retroreflective, highly compatible with line paint. especially &p glass beads can be obtained.
Bulusun Çözümünü Amaçladigi Teknik Problem Yollarda gündüzleri rahatlikla görülebilen yol çizgileri, gece karanlikta görünür olmalarini yüzeylerinde bulunan cam kürelerine borçludur. Cam küreler küresel seklinin ve cam yapisinin etkisiyle, gece araçlardan yol çizgilerine gelen far isiklarini geri yansitarak sürücüye yatay isaretleri görünür kilmaktadir. Bu da sürücünün yol çizgileri sayesinde yönlendirilmesine ve daha dikkatli, trafik kurallarina uygun bir yolculuk yapmasina yardimci olmaktadir. Cam küreler; yagmurlu havada bile far isigini geri yansitabildikleri için, geceleri trafik güvenligini saglamak açisindan önemlidir. Bu sekilde gelen isigin isik kaynagina geri yansitilmasina boya içindeki yüzdesi, hacimce boya yüzeyinde kalacak kismi, retroreflektivite en yüksek düzeyde olacak sekilde ayarlanmaktadir. The Technical Problem That The Invention Aims To Solve Road lines, which can be easily seen on the roads during the day, are visible in the dark at night. They owe their existence to the glass spheres on their surfaces. glass spheres spherical With the effect of its shape and glass structure, the headlights coming from the vehicles to the road lines at night reflects back, making horizontal markings visible to the driver. This is the driver's way lines and a more careful, traffic-compliant It helps him travel. glass spheres; even in the rain Since they can reflect the light back, they are used to ensure traffic safety at night. is important. In this way, the incoming light is reflected back to the light source. the percentage in the paint, the part that will remain on the paint surface by volume, the retroreflectivity is set at a high level.
Yol çizgi boyalarinin üzerinden araçlar geçtikçe boyaya tutunmus olan farkli gradasyondaki cam kürelerin yüzeyde bulunan büyük tane boyutlulari araçlarin yapmis oldugu sürtünme etkisiyle yüzeyden ayrilmakta ve küçük tane boyutlular boyanin da zamanla asinmasina bagli olarak yüzeye dogru çikmaktadirlar. Sonuçta da, gece görünürlülügü zaman içinde azalmaktadir. Gece görünürlülügünün uzun süreli olmasi için cam küre ile boya arasinda siki bir bag olmalidir. Bunu saglayabilmek için de cam küreler, bu bagi saglayabilecek farkli malzemelerle kaplanmaktadirlar [1,2,3]. Literatürde bunu saglayabilmek için genellikle organik esasli polimerik yapiya sahip malzemeler tercih edilmistir. Bu tür malzemelerin yapilari boya malzemesi içinde bulunan baglayici ile uygun kimyasal yapida olmalidir ki uygulama sirasinda yol çizgi boyasi üzerine atilan cam küreciklerin bir kismi yukarida kalirken bir kismi da boyaya batmadan durabilecek sekilde yapisma islemi gerçeklestirilmelidir. Yani kaplama malzemesinin kimyasal yapisi boya içinde bulunan baglayiciya yapisacak sekilde seçilmelidir. Bu tür malzemelerde ayrica zamanla günesin etkisiyle sararma problemleri olabildigi gibi hava sicakliginin artmasina bagli olarak cam kürecik üzerinde bulunan kaplamalarda organik esasli bazi bilesenlerin difüzyonu gibi problemler de yasanabilmektedir. As vehicles pass over the road marking paints, different paints are attached to the paint. The large grain sizes of the glass spheres in the gradation It is separated from the surface by the effect of friction and small grain sizes they rise towards the surface depending on the wear of the paint over time. After all Also, visibility at night decreases over time. Long night visibility For it to last, there must be a tight bond between the glass ball and the paint. this much In order to provide this bond, glass spheres are made with different materials that can provide this bond. they are covered [1,2,3]. In order to provide this in the literature, organic Materials with based polymeric structure are preferred. Such materials Their structure should be in a chemical structure suitable for the binder in the paint material. Some of the glass beads thrown on the road marking paint during two applications The process of sticking in such a way that a part of it can stand without sinking into the paint while remaining above should be carried out. In other words, the chemical structure of the coating material is in the paint. It should be selected to stick to the connector found. In such materials, There may be yellowing problems with the effect of the sun over time, as well as the air temperature. organic-based coatings on the glass bead depending on the increase in Problems such as diffusion of some components can also be experienced.
Bu bulusta cam küreler, inorganik esasli, nanoboyutlu dogal sodyum montmorillonit ve kuaterner amonyum tuzlari ile modifiye edilmis montmorillonit örnekleriyle kaplanmistir. Daha sonra, kaplanmamis veya ticari olarak su bazli yol çizgi boya uygulamalarinda önemli bir yere sahip silan esasli polimerik malzemelerle kapli cam kürelerle performans açisindan kiyaslanmistir. Performans testleri sonrasinda daha daha uzun ömürlü bir uygulama olanagi saglanmistir. Ayrica ilgili kaplama malzemesinin inorganik esasli dogal bir ürün olmasina bagli olarak zamanla yasanabilecek difüzyon problemleri engellenirken daha ucuz maliyetler söz konusudur. Kaplamada kullanilan malzemenin simdiye kadar bu amaçla ilk kez bu çalisma ile kullanilmis olmasi, dogal kaynaklarin katma degeri yüksek ürünlere dönüstürülmesi açisindan da ayrica bir öneme sahiptir. Üstün geri yansitma özelliginin ve yüksek asinma direncinin yanisira yukarida belirtilen tüm özellikleri nedeniyle bu bulus diger patentlerden farklilik arz etmektedir. In this invention, glass spheres are inorganic based, nanosized natural sodium montmorillonite. and montmorillonite samples modified with quaternary ammonium salts. is covered. Next, uncoated or commercially water-based road marking paint Glass coated with silane-based polymeric materials, which have an important place in Compared to spheres in terms of performance. After performance tests a longer lasting application opportunity is provided. Related coating over time, depending on the fact that the material is an inorganic based natural product. While preventing diffusion problems that may occur, cheaper costs are promised. subject. This is the first time that the material used in the coating has been used for this purpose until now. The fact that it has been used with work, natural resources to products with high added value. It is also important in terms of conversion. Superior reflectivity In addition to its feature and high wear resistance, all the above-mentioned features Therefore, this invention differs from other patents.
Sekillerin Açiklamasi Sekillerde kullanilan kisaltmalar asagidaki sekilde tanimlanmaktadir: MMT-1 Sodyum montmorillonitin katyon degistirme kapasitesine es oranda kuaterner amonyum tuzu kullanilarak modifiye edilen kil MMT-2 Sodyum montmorillonitin katyon degistirme kapasitesinin yaklasik 2 kati oraninda kuaterner amonyum tuzu kullanilarak modifiye edilen kil MMT-3 Zenginlestirilmis sodyum montmorillonit * CK-1 : Kaplamasiz cam küre CK-2 : Silan kaplamali cam küre CK-3 : Sodyum montmorillonitin katyon degistirme kapasitesine es oranda kuaterner amonyum tuzu kullanilarak modifiye edilen kil ile kaplanan cam küre CK-4 : Sodyum montmorillonitin katyon degistirme kapasitesinin yaklasik 2 kati oraninda kuaterner amonyum tuzu kullanilarak modifiye edilen kil ile kaplanan cam küre CK-5 : Zenginlestirilmis sodyum montmorillonit ile kapli cam küre Sekil 1. FT-IR Infrared Spektoskopisinde, O-H esneme titresim frekansi boyunda oktahedral tabakaya ait pik daha belirgin gözükmektedir. Bu pikler montmorilloniti göstermektedir. MMT-1 ve MMT-2 ait FT-IR sonuçlari birbirine FT-IR sonucunda görülmeyen pikler vermektedir. 2950-2850 cm-1 dalga boylarindaki piklerin metilen yapisini, 1470-1370 cm`1 dalga boylarindaki piklerin H-C-H titresimlerini gösterdigi göz önüne alindiginda organik yapinin varligi, yani kuaterner amonyum tuzu varligi ortaya çikmaktadir. Description of Figures The abbreviations used in the figures are defined as follows: Equal to the cation exchange capacity of MMT-1 Sodium montmorillonite clay modified using quaternary ammonium salt The cation exchange capacity of MMT-2 Sodium montmorillonite is approximately 2 clay modified using a solid ratio of quaternary ammonium salt MMT-3 Enriched sodium montmorillonite * CK-1 : Uncoated glass ball CK-2 : Silane coated glass ball CK-3 : Equal to the cation exchange capacity of sodium montmorillonite glass sphere coated with clay modified using quaternary ammonium salt CK-4 : The cation exchange capacity of sodium montmorillonite is approximately 2 with clay modified using a solid proportion of quaternary ammonium salt coated glass ball CK-5 : Glass sphere coated with enriched sodium montmorillonite Figure 1. O-H stretch vibration frequency in FT-IR Infrared Spectoscopy The peak of the octahedral layer appears more prominent in the neck. These peaks indicates montmorillonite. FT-IR results of MMT-1 and MMT-2 It gives peaks that are not seen in the FT-IR result. at wavelengths of 2950-2850 cm-1 the methylene structure of the peaks, the peaks at 1470-1370 cm`1 wavelengths, H-C-H the existence of organic structure, that is, quaternary the presence of ammonium salt is revealed.
Sekil 2. TGAýEgisigdejnalizleri gerçeklestirilÄnumunelerin TGA sonuçlarinda O- 150 °C arasinda görülen düsüs, kil minerallerinin tabakalari arasindaki suyun safsizliklar ile OH iyonlari yapidan uzaklasmistir. Modifiye kile ait isil analizlerinden elde edilen TGA egrilerinde, 200 °C-400°C arasinda görülen düsüs ise (MMT-1 ve MMT-2 için), amonyum tuzunun yapiya girdigini ve karbonun yandigini göstermektedir. ' Sekil 3. SEM (Taramali Elektron Mikroskobu - Scanning Electron Microscope) Fotograflari, (a) CK-1, (b) CK-3, (c) CK-4, (d) CK-5 görüntülerinde cam küreciklerin MMT ile kaplandigi görülmektedir. MMT-2 ile kapli cam küreciklerinde gözlenenen parlakligin nedeni yüksek oranda kullanilan kuaterner amonyum tuzudur. Figure 2. TGAİEgisigdejnalysis of the samples was found in the TGA results of O- The decrease observed between 150 °C is that the water between the layers of clay minerals impurities and OH ions were removed from the structure. Thermal analyzes of modified clay In the TGA curves obtained, the decrease observed between 200 °C-400 °C (MMT-1 and For MMT-2), the ammonium salt enters the structure and the carbon is burned. shows. ' Figure 3. SEM (Scanning Electron Microscope) Photographs of (a) CK-1, (b) CK-3, (c) CK-4, (d) CK-5 In the images, it is seen that the glass beads are coated with MMT. coated with MMT-2 The brightness observed in the glass beads is due to the highly used quaternary is the ammonium salt.
Bulusun Açiklanmasi Kaplama Çalismalari Cam kürelerin dogal montmorillonit ile kaplanmasi çalismasinda ilk asamada montmorillonit (MMT) süspansiyonu hazirlanmistir. Zenginlestirilmis ve katyon degistirme kapasitesi (KDK) 105 meq/1OO gr olan montmorillonit kullanarak MMT/süspansiyon orani % 0.5-2 olacak sekilde su içerisinde 30-80°C'de dagilmasi (dispersiyon) saglanmis ve homojen bir süspansiyon elde edilmistir. Daha sonra cam küre/ MMT süspansiyon orani 1:1-1:4 arasinda olacak sekilde cam küre, önceden hazirlanan MMT/ su süspansiyonuna dahil edilmis ve kisa bir süre karistirilmistir. Bu islem sonucunda kaplama kalinligi 0,1-0,5 mikron arasinda olmaktadir. Bu karisim, cam kürelerin iyice yayilabilecegi bir sekilde tava içerisine alinmis ve 80-100°C sicaklik araliginda kurutulmustur. Kurutma islemi sonrasinda topaklanmalari gidermek için ögütücü içinde çok hafif bir sekilde ögütme ile cam kürelerin birbirinden ayrilmasi saglanmistir. Bu islem sirasinda cam kürelerin kirilmamasina özen gösterilmelidir. Disclosure of the Invention Coating Works In the first stage of the study of coating glass spheres with natural montmorillonite, montmorillonite (MMT) suspension was prepared. Enriched and cation using montmorillonite with a replacement capacity (KDK) of 105 meq/1OO gr. Disperse in water at 30-80°C with a MMT/suspension ratio of 0.5-2% (dispersion) was provided and a homogeneous suspension was obtained. Then the glass The glass ball should be pre-washed with a suspension ratio of 1:1-1:4 to the ball/MMT. It was included in the prepared MMT/water suspension and stirred for a short time. This As a result of the process, the coating thickness is between 0.1-0.5 microns. This is my mix It was taken into the pan in such a way that the glass spheres could spread well and at 80-100°C. dried in the temperature range. Agglomeration after drying to remove the glass balls from each other by grinding very lightly in the grinder. separation is ensured. Take care not to break the glass spheres during this process. should be displayed.
Modifiye montmorillonit ile kaplama isleminde ise yukarida belirtilen sekilde su içinde disperse edilen MMT'ye ilave olarak MMT'nin katyon degistirme kapasitesinin yarisi, katyon degistirme kapasitesine esit ve katyon degistirme kapasitesinin yaklasik 2 kati olacak sekilde kuaterner amonyum tuzu eklenmistir. Süspansiyon 30-80 °C sicaklikta 0.5-2 saat karistirildiktan sonra yukaridaki gibi kaplama ve kurutma islemleri gerçeklestirilmistir. In the coating process with modified montmorillonite, it is soaked in water as stated above. half the cation exchange capacity of MMT in addition to the dispersed MMT, Equal to the cation exchange capacity and about 2 times the cation exchange capacity Quaternary ammonium salt was added as Suspension at a temperature of 30-80 °C After mixing for 0.5-2 hours, coating and drying processes as above has been carried out.
Kaplanan cam küreler briket üzerine çekilmis boyaya agirlikça % 33 oraninda serpilmistir. Cam kürelerin üzerine atildigi boyalar su bazli baglayicilardan olusan su bazli yol çizgi boyalaridir. Briketler üzerine çekilen boya filmlerinin yas film kalinligi 400-600 mikron arasindadir. Boya üzerine serpilen cam küreler farkli gradasyonda olup, bu cam kürelerin tane boyutu ise 150-700 mikron aralaginda degismektedir. The coated glass spheres add 33% by weight to the applied paint on the briquette. sprinkled. The paints on which the glass spheres are applied are water-based binders. based road marking paints. Wet film thickness of paint films shot on briquettes It is between 400-600 microns. Glass spheres sprinkled on paint in different gradation and the grain size of these glass spheres varies in the range of 150-700 microns.
Boya kuruduktan sonra yolu simüle etmek amaciyla 6 bar basinç uygulayacak sekilde bir adet tekerlek boya üzerinde gidip gelmistir. Her bir gidip gelme 1 devir sayilmistir ve 10.000 devire kadar bu islem sürdürülmüstür. After the paint dries, it will apply 6 bar pressure to simulate the road. In this way, one wheel went back and forth on the paint. 1 cycle per commute counted and this process was continued until 10,000 cycles.
Karakterizasyon FT-IR Infrared Spektoskopisi Cam kürelerin kaplandigi MMT'Ierin FT-IR infrared Spektoskopisi, dogal montmorillonit ve modifiye montmorillonitin belirtilmesi amaciyla Perkin Elmer Termal Gravimetrik Analiz (TGA) Cam kürelerin kaplandigi MMT7lerin termal gravimetrik analizi, dogal montmorillonit ve modifiye montmorillonitin gösterilmesi amaciyla Perkin Elmer Pyris 1 model cihaz ile 950°C'ye kadar isitilarak gerçeklestirilmistir (Sekil 2) Scanning Electron Mikroskop (SEM) Kaplanan cam kürelerin morfolojik incelemesi JEOL 6335F marka elektron mikroskobu kullanilarak gerçeklestirilmistir (Sekil 3) Cam küreciklerin mikroskop görüntüleri ise Sekil 4'te verilmistir. Characterization FT-IR Infrared Spectoscopy FT-IR infrared Spectoscopy of MMTs coated with glass spheres, natural Perkin Elmer for the designation of montmorillonite and modified montmorillonite Thermal Gravimetric Analysis (TGA) Thermal gravimetric analysis of MMT7s coated with glass spheres, natural montmorillonite and Perkin Elmer Pyris 1 model device for demonstration of modified montmorillonite by heating up to 950°C (Figure 2) Scanning Electron Microscope (SEM) Morphological examination of coated glass spheres JEOL 6335F brand electron carried out using a microscope (Figure 3) Microscopic images of the glass beads are given in Figure 4.
Cam Küre Performans Testi Cam küre performansini ölçmek için tekerlek altinda asinma testi uygulanmis ve belli düzeylerde asinmaya ugrayan örneklerde gece görünürlülük degerleri ölçülmüstür. Glass Globe Performance Test In order to measure the glass ball performance, a wear test was applied under the wheels and a certain Visibility values at night were measured on the samples that were eroded at high levels.
Yol simülasyonu saglayan bu test sonucunda gece görünürlülügü degerleri ölçülmüstür. Su bazli yol çizgi boyasi ile birlikte kullanilan cam küreler su sekildedir : CK-1 : Kaplamasiz cam küre CK-2 : Silan kapli ticari cam küre CK-3 : 221 Modifiye montmorillonit CK-4 : 121 Modifiye montmorillonit CK-5 : 0,5:1 Modifiye montmorillonit CK-6 : Na-montmorillonit Arazi uygulamalarinda oldugu gibi boya 600 mikron yas film kalinliginda olmak üzere briketler üzerine çekilmistir. Yol çizgi boyasi üzerinde cam küreciklerin görüntüsü Sekil 5'te verilmistir. 6 bar civarinda basinç uygulayan tekerlek briket üzerinde gidip gelmekwgelme 1 devir sayi_lm_aktadir. 10.000 .devire .kadar gece görünürlülük degerleri ölçülmüstür (Tablo 1) Sonuçlar incelendiginde 1000 devir sonunda cam küre olarak silan kapli ticari ürün CK-2 içeren boya en yüksek gece görünürlülügü degerine sahip iken 3000 devirde sodyum montmorillonit kapli cam küre CK-5 içeren boyanin gece görünürlülük degeri CK-2 içeren boyanin gece görünürlülük degeri ile esit hale gelmis ve 10.000 devire kadar aradaki fark CK-5 lehinde artmistir. Bu durum CK-5'in boyaya yapismasinin ticari üründen iyi oldugunu göstermektedir. Tekerlek geçtikçe boya asinmakta ve boya asinirken alttan yeni cam küreler çikmaktadir. Bu islem sonunda diger cam küreler boya yüzeyinden koparken CK-5”in kopmasi daha az olmakta ve 8.000 devire kadar gece görünürlülügü CK-S içeren boyada artmaktadir. 10.000 devirden sonra degerler düsmesine ragmen CK-5 içeren boyanin gece görünürlülügü CK-2 içeren boyanin yaklasik 1,5 katidir. CK-3 ve CK-4 içeren boyalarin gece görünürlülük degerleri kaplamasiz cam küre CK-1 içeren boyanin gece görünürlülük degerlerinden daha yüksektir. As a result of this test, which provides road simulation, night visibility values has been measured. Glass spheres used with water-based road marking paint are as follows: CK-1 : Uncoated glass ball CK-2 : Silane coated commercial glass ball CK-3 : 221 Modified montmorillonite CK-4 : 121 Modified montmorillonite CK-5 : 0.5:1 Modified montmorillonite CK-6 : Na-montmorillonite As in field applications, the paint is 600 micron wet film thickness. drawn on briquettes. Image of glass beads on road marking paint It is given in Figure 5. The wheel, which exerts a pressure of around 6 bar, goes on the briquette. to comewgeme is 1 cycle count_lm_akta. night up to 10,000 cycles visibility values were measured (Table 1). When the results are examined, 1000 cycles The paint containing the silane-coated commercial product CK-2 as a glass sphere at the end Sodium montmorillonite coated glass at 3000 rpm The nighttime visibility value of the spherical CK-5-containing paint It has become equal with the visibility value and the difference up to 10,000 revolutions is CK-5 increased in favor. This indicates that the adhesion of CK-5 to the paint is better than the commercial product. shows. The paint wears off as the wheel goes on, and as the paint wears off, new glass from below spheres come out. At the end of this process, while the other glass spheres break off from the paint surface, The CK-5 has less breakage and night visibility up to 8,000 rpm. increases in dye containing Although the values decrease after 10,000 cycles, the CK-5 The night visibility of the paint containing CK-2 is approximately 1.5 times that of the paint containing CK-2. CK-3 and Night visibility values of CK-4-containing paints are uncoated glass ball CK-1-containing It is higher than the night visibility values of the paint.
Tablo 1. Gündüz ve Gece Görünürlülügü Numuneadi Rl Qd Rl Qd Rl Qd Rl Qd Rl Qd Rl Qd * RI : Gündüz Görünürlülügü ; Qd : Gece görünürlülügü Bulusun Sanavive Uvqulanma Biçimi Üretilen veya satin alinan cam küreler, bentonit süspansiyonu içerisinde ortam sicakliginda karistirilacaktir. Karistirma isleminden sonra kapli cam küreler kurutulacaktir. Kurutma islemi cam kürelerin birbirine yapismasini engelleyecek sekilde akiskan yatakta yapilabilecegi gibi sabit kurutmadan sonra hafif darbe ile yapisan cam küreler kirilmadan birbirinden ayrilir. Bu haliyle cam küreler, yol çizgi boyalarinda kullanima hazir haldedir. Table 1. Day and Night Visibility Sample name Rl Qd Rl Qd Rl Qd Rl Qd Rl Qd Rl Qd * RI : Day Visibility ; Qd : Night visibility How the Invention Is Applied Produced or purchased glass spheres, medium in bentonite suspension It will be mixed at the temperature. Coated glass spheres after mixing it will be dried. The drying process will prevent the glass spheres from sticking to each other. It can be done in a fluidized bed as well as with a light blow after constant drying. The adhered glass spheres are separated from each other without breaking. As such, the glass spheres, the road line It is ready for use in paints.
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TR2014/11519A TR201411519A2 (en) | 2014-09-30 | 2014-09-30 | Improvements in surface properties of the glass beads which are used as retrorefrective material in road markings by coating with natural clay |
CN201580052963.9A CN107148405B (en) | 2014-09-30 | 2015-09-30 | Surface property improvement of glass beads for use as retroreflective material in pavement markings by natural clay coating |
JP2017517049A JP6381793B2 (en) | 2014-09-30 | 2015-09-30 | Method for producing glass beads coated with montmorillonite and / or modified montmorillonite |
PCT/IB2015/057487 WO2016051354A1 (en) | 2014-09-30 | 2015-09-30 | Improvements in surface properties of the glass beads which are used as retrorefrective material in road markings by coating with natural clay |
RU2017108722A RU2661511C1 (en) | 2014-09-30 | 2015-09-30 | Improvement of surface properties of glass beads used as light-reducing material for road marking, by natural clay covering |
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GB8508093D0 (en) | 1985-03-28 | 1985-05-01 | Glaverbel | Modifying wettability of glass beads |
LU86880A1 (en) | 1987-05-14 | 1989-01-19 | Glaverbel | GLASS MICROBALLS INTENDED TO BE IN CONTACT WITH POLYMERIZABLE MATERIALS; PROCESS FOR TREATING GLASS MICROBALLS TO MAKE THEM SUITABLE FOR USE AND POLYMERIZATION METHOD USING SUCH MICROBILLES |
LU87138A1 (en) * | 1988-02-19 | 1989-09-20 | Glaverbel | SURFACE-TREATED GLASS BEADS, METHOD FOR TREATING THE SURFACE OF GLASS BEADS, AND SYNTHETIC POLYMER MATRIX INCORPORATING SUCH GLASS BEADS |
US5077117A (en) * | 1990-04-05 | 1991-12-31 | Minnesota Mining And Manufacturing Company | Pavement marking material with rupturing top layer |
JPH07295487A (en) * | 1994-04-27 | 1995-11-10 | Aisin Chem Co Ltd | Photo-recursive reflecting paint film, and its formation method |
AU1852401A (en) | 1999-12-10 | 2001-06-18 | Abildgaard Roadvision Aps | A reflective road marking and a method of producing and applying a reflective road marking composition |
JP2003268311A (en) * | 2002-03-15 | 2003-09-25 | Seitoo Kk | Road marking paint |
MXPA06004844A (en) | 2003-11-06 | 2006-07-06 | 3M Innovative Properties Co | Retroreflective elements comprising a bonded resin core and pavement markings. |
US20050158461A1 (en) * | 2004-01-21 | 2005-07-21 | 3M Innovative Properties Company | Methods of making reflective elements |
CN100513311C (en) * | 2005-11-04 | 2009-07-15 | 浙江海力生制药有限公司 | Modified smectite and method for producing the same and its application |
US7563508B2 (en) * | 2007-05-30 | 2009-07-21 | Chung Shan Institute Of Science And Technology, Armaments Bureau, M.N.D. | Diffusion beads with core-shell structure |
RU2422269C1 (en) * | 2010-03-17 | 2011-06-27 | Государственное образовательное учреждение высшего профессионального образования "Тверской государственный технический университет" | Method of producing road cover plate |
JP2015148115A (en) * | 2014-02-07 | 2015-08-20 | 株式会社キクテック | Paint for road surface line sign and road surface line sign |
-
2014
- 2014-09-30 TR TR2014/11519A patent/TR201411519A2/en unknown
-
2015
- 2015-09-30 RU RU2017108722A patent/RU2661511C1/en active
- 2015-09-30 WO PCT/IB2015/057487 patent/WO2016051354A1/en active Application Filing
- 2015-09-30 CN CN201580052963.9A patent/CN107148405B/en not_active Expired - Fee Related
- 2015-09-30 JP JP2017517049A patent/JP6381793B2/en not_active Expired - Fee Related
Also Published As
Publication number | Publication date |
---|---|
JP2018501170A (en) | 2018-01-18 |
JP6381793B2 (en) | 2018-08-29 |
CN107148405A (en) | 2017-09-08 |
WO2016051354A1 (en) | 2016-04-07 |
CN107148405B (en) | 2019-12-31 |
RU2661511C1 (en) | 2018-07-17 |
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