KR20120043580A - Near-infrared absorption material and manufacturing method of the same - Google Patents
Near-infrared absorption material and manufacturing method of the same Download PDFInfo
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- KR20120043580A KR20120043580A KR1020100104939A KR20100104939A KR20120043580A KR 20120043580 A KR20120043580 A KR 20120043580A KR 1020100104939 A KR1020100104939 A KR 1020100104939A KR 20100104939 A KR20100104939 A KR 20100104939A KR 20120043580 A KR20120043580 A KR 20120043580A
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- Prior art keywords
- compound
- infrared absorber
- copper
- neodymium
- infrared
- Prior art date
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 title description 12
- 239000000463 material Substances 0.000 title description 3
- 239000006096 absorbing agent Substances 0.000 claims abstract description 58
- 239000000203 mixture Substances 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000005749 Copper compound Substances 0.000 claims abstract description 23
- 150000001880 copper compounds Chemical class 0.000 claims abstract description 23
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 19
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 150000003018 phosphorus compounds Chemical class 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims description 22
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- -1 phosphorus compound Chemical class 0.000 claims description 13
- 229910052698 phosphorus Inorganic materials 0.000 claims description 11
- 239000011574 phosphorus Substances 0.000 claims description 11
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 239000003973 paint Substances 0.000 claims description 9
- 230000002745 absorbent Effects 0.000 claims description 8
- 239000002250 absorbent Substances 0.000 claims description 8
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 4
- 239000005750 Copper hydroxide Substances 0.000 claims description 4
- 229910001956 copper hydroxide Inorganic materials 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 239000005751 Copper oxide Substances 0.000 claims description 2
- 229910000431 copper oxide Inorganic materials 0.000 claims description 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- YWEUIGNSBFLMFL-UHFFFAOYSA-N diphosphonate Chemical compound O=P(=O)OP(=O)=O YWEUIGNSBFLMFL-UHFFFAOYSA-N 0.000 claims description 2
- CFYGEIAZMVFFDE-UHFFFAOYSA-N neodymium(3+);trinitrate Chemical compound [Nd+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O CFYGEIAZMVFFDE-UHFFFAOYSA-N 0.000 claims description 2
- ATINCSYRHURBSP-UHFFFAOYSA-K neodymium(iii) chloride Chemical compound Cl[Nd](Cl)Cl ATINCSYRHURBSP-UHFFFAOYSA-K 0.000 claims description 2
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 2
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims 1
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims 1
- 229940075624 ytterbium oxide Drugs 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002341 toxic gas Substances 0.000 abstract description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000040 hydrogen fluoride Inorganic materials 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- 239000012153 distilled water Substances 0.000 abstract description 2
- 150000003748 yttrium compounds Chemical class 0.000 abstract 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract 1
- 239000000976 ink Substances 0.000 description 27
- 239000010949 copper Substances 0.000 description 8
- 239000000975 dye Substances 0.000 description 8
- 235000011007 phosphoric acid Nutrition 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 7
- 229910052802 copper Inorganic materials 0.000 description 7
- 239000000049 pigment Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 239000002966 varnish Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 239000002574 poison Substances 0.000 description 4
- 231100000614 poison Toxicity 0.000 description 4
- 238000007650 screen-printing Methods 0.000 description 4
- 238000001392 ultraviolet--visible--near infrared spectroscopy Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 229910021594 Copper(II) fluoride Inorganic materials 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- GWFAVIIMQDUCRA-UHFFFAOYSA-L copper(ii) fluoride Chemical compound [F-].[F-].[Cu+2] GWFAVIIMQDUCRA-UHFFFAOYSA-L 0.000 description 2
- 150000002798 neodymium compounds Chemical class 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- RILZRCJGXSFXNE-UHFFFAOYSA-N 2-[4-(trifluoromethoxy)phenyl]ethanol Chemical compound OCCC1=CC=C(OC(F)(F)F)C=C1 RILZRCJGXSFXNE-UHFFFAOYSA-N 0.000 description 1
- MJFITTKTVWJPNO-UHFFFAOYSA-N 3h-dithiole;nickel Chemical class [Ni].C1SSC=C1 MJFITTKTVWJPNO-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 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
- 230000008033 biological extinction Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000000018 nitroso group Chemical group N(=O)* 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- ANRHNWWPFJCPAZ-UHFFFAOYSA-M thionine Chemical compound [Cl-].C1=CC(N)=CC2=[S+]C3=CC(N)=CC=C3N=C21 ANRHNWWPFJCPAZ-UHFFFAOYSA-M 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 150000003747 ytterbium compounds Chemical class 0.000 description 1
- KUBYTSCYMRPPAG-UHFFFAOYSA-N ytterbium(3+);trinitrate Chemical compound [Yb+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O KUBYTSCYMRPPAG-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
Abstract
Description
본 발명은 근적외선을 흡수하는 특성을 가진 비가시광 흡수제 및 그 제조방법에 관한 것으로, 더욱 상세하게는 구리 화합물; 인화합물; 및 네오디늄 또는 이터비움 화합물을 포함하는 700 내지 1300nm의 파장을 흡수하는 근적외선 흡수제 및 그 제조방법에 관한 것이다.
The present invention relates to an invisible light absorbing agent having a property of absorbing near infrared rays, and a method of manufacturing the same, and more particularly, to a copper compound; Phosphorus compounds; And a near-infrared absorber absorbing a wavelength of 700 to 1300 nm including a neodymium or an etherium compound, and a method of manufacturing the same.
종래의 인쇄기술은 육안으로 식별이 가능한 가시광 영역의 도료나 잉크를 사용하여 물체나 화상을 표현해 왔기 때문에, 보안문서 등의 특수인쇄물에 적용하는 경우 매우 정밀한 공정을 통한 세밀한 화상의 표현이나 인쇄물 자체의 특성을 이용하여 위조, 변조의 가능성을 배제시키기 위한 노력을 해왔다. Conventional printing technology has expressed objects or images using paint or ink in the visible region that can be visually identified. Therefore, when applied to special prints such as security documents, the detailed printing of the print or the print itself Efforts have been made to rule out the possibility of forgery and modulation using features.
이후 비가시광 영역을 흡수하거나 반사시키는 물질을 이용한 염료나 안료가 개발되면서, 가시광선 영역은 반사하고 비가시광 영역은 일부분 흡수하는 구성을 통하여 보안문서의 진위 여부를 식별하도록 함으로써, 보안 문서의 위조, 변조를 방지할 수 있는 기술이 급속도로 발전하고 있다. Since the development of dyes or pigments using a material that absorbs or reflects the invisible light region, by identifying the authenticity of the security document through the configuration that reflects the visible light region and partially absorbs the invisible region, forgery of the security document, Techniques for preventing tampering are rapidly evolving.
그러나, 일반적인 염료나 안료는 가시광선의 특정파장을 부분적으로 흡수 또는 반사하지만, 적외선 영역에서의 흡수 또는 반사 특성이 가시광선과 일치하지 않으며, 대부분의 염료나 안료들은 적외선에 대해서는 강한 흡수를 하지 않는다.However, general dyes or pigments partially absorb or reflect specific wavelengths of visible light, but absorption or reflection characteristics of the infrared region do not coincide with visible light, and most dyes or pigments do not have strong absorption of infrared light.
종래의 염료나 안료 중에 적외선을 흡수하는 물질로는 카본블랙, 프탈로시아닌블루, 니트로소계 염료, 시아닌계 염료, 니그로신계 염료, 트리페닐메탄계 염료와 금속의 착화합물인 니켈디티올렌계 등이 있지만, 고유의 색상이 강하여 잉크 조성물로 사용할 경우 원하는 색상을 얻지 못하였다. In general, dyes and pigments that absorb infrared light include carbon black, phthalocyanine blue, nitroso-based dyes, cyanine-based dyes, nigrosine-based dyes, triphenylmethane-based dyes, and nickel dithiolenes, which are complexes of metals. When the color of the strong used as an ink composition did not obtain the desired color.
이를 개선하기 위한 노력으로, 일본 특개평 5-279078호에는 무색에 가까운 미청색의 물질로서 구리 화합물과 인화합물이 근적외선을 흡수하는 효과가 있음을 개시하였다. In an effort to improve this, Japanese Patent Laid-Open No. Hei 5-279078 discloses that the copper compound and the phosphorus compound absorb the near infrared rays as a colorless, light blue material.
또한, 일본 특개평 6-207161호에서는 구리계 근적외선 흡수제를 제조함에 있어 코발트, 마그네슘, 칼슘, 스트론튬, 바륨 등을 첨가하는 기술을 개시하였지만, 이 경우 근적외선 흡수제의 담색화에 기여하는데 그쳤고, 근적외선 흡수능을 개선하지는 못하였다. In addition, Japanese Patent Laid-Open No. 6-207161 discloses a technique of adding cobalt, magnesium, calcium, strontium, barium, etc. in the preparation of a copper-based near infrared absorber, but in this case, it contributed to the lightening of the near infrared absorber. It did not improve.
대한민국공개특허공보 제2002-0058117호에는 사불화 붕산구리와 인산 등으로 구성되며 미청색을 나타내면서 몰 흡광계수가 더욱 우수한 적외선 흡수제를 기재하고 있으나 소성 후에 입자화가 어려운 문제점을 가지고 있다.Korean Laid-Open Patent Publication No. 2002-0058117 discloses an infrared absorber composed of copper tetrafluoroborate, phosphoric acid, and the like, which has a light blue color, and which has a better molar extinction coefficient, but has a problem of difficult granulation after firing.
대한민국공개특허공보 제2005-0085074호에는 사불화붕산구리, 인산 및 붕산을 사용하여 발포시킴으로서 무색에 가까우면서 입자화가 용이한 비가시광 흡수제의 제조방법이 기재되어 있으나, 불화수소와 같은 유독가스가 발생되는 문제점이 있다.Korean Laid-Open Patent Publication No. 2005-0085074 describes a method for preparing an invisible light absorber that is close to colorless and easily granular by foaming with copper tetrafluoroborate, phosphoric acid and boric acid, but generates toxic gases such as hydrogen fluoride. There is a problem.
또한, 구리계 근적외선 흡수제는 백색이면서 근적외선을 흡수하는 특성이 있어 보안 잉크 등으로 사용할 수 있지만 근적외선 흡수능력을 충분히 발휘하기 위해서는 제조 잉크의 약 40% 이상의 함량이 첨가되어야 하기 때문에, 근적외선 흡수능력을 향상시켜 보안 잉크 제조 시에 근적외선 흡수제의 함량을 낮출 수 있도록 하는 노력이 계속되어 왔다. In addition, the copper-based near infrared absorber is white and absorbs near infrared rays, so that it can be used as a security ink. However, in order to fully exhibit near infrared absorption ability, a content of about 40% or more of the manufactured ink must be added, thereby improving near infrared absorption ability. Efforts have been made to reduce the content of near-infrared absorbers in the manufacture of security inks.
이에, 본 발명자들은 상기 문제점을 해결하기 위하여 예의 노력한 결과, 구리계 근적외선 흡수제의 제조시 증류수와 알코올을 혼합 사용하고, 네오디늄 또는 이터비움 화합물을 첨가하는 경우, 근적외선 흡수능력이 향상되고 입자의 응집을 막을 수 있다는 것을 확인하고, 본 발명을 완성하게 되었다.
Therefore, the present inventors have made diligent water and alcohol when preparing a copper-based near-infrared absorber, and when the neodymium or iterium compound is added, the near-infrared absorption is improved and the particles are aggregated. It was confirmed that the present invention can be prevented, and the present invention was completed.
본 발명의 목적은 구리화합물; 인화합물; 및 네오디늄 또는 이터비움 화합물을 포함하고 700 ~ 1300nm의 근적외선 파장을 흡수하는 근적외선 흡수제 및 그 제조방법을 제공하는데 있다. An object of the present invention is a copper compound; Phosphorus compounds; And a near-infrared absorber containing neodymium or an etherium compound and absorbing a near infrared wavelength of 700 to 1300 nm, and a method of manufacturing the same.
본 발명의 다른 목적은 상기 근적외선 흡수제를 함유하는 잉크 조성물 및 페인트 조성물을 제공하는데 있다.
Another object of the present invention is to provide an ink composition and a paint composition containing the near infrared absorber.
상기 목적을 달성하기 위하여, 본 발명은 구리화합물; 인화합물; 및 네오디늄 또는 이터비움 화합물을 포함하는 근적외선 흡수제를 제공한다. In order to achieve the above object, the present invention is a copper compound; Phosphorus compounds; And a near infrared absorber comprising neodymium or an iterium compound.
본 발명은 또한, 에탄올 수용액에 구리화합물, 인화합물 및 네오디늄 또는 이터비움 화합물을 혼합하여 실온에서 교반, 여과 및 수세 후 건조시키는 단계; 상기 혼합물을 전기로에 넣어 서서히 가열하면서 소성하는 단계; 및 상기 소성된 혼합물을 분쇄하여 입자화하는 단계를 포함하는 근적외선 흡수제의 제조방법을 제공한다. The present invention also comprises the steps of mixing a copper compound, a phosphorus compound and a neodymium or etherium compound in an aqueous solution of ethanol at room temperature after stirring, filtration and washing with water; Sintering the mixture into an electric furnace and slowly heating it; And it provides a method for producing a near-infrared absorber comprising the step of pulverizing the calcined mixture.
본 발명은 또한, 상기 근적외선 흡수제를 포함하는 잉크 조성물 및 페인트 조성물을 제공한다.
This invention also provides the ink composition and paint composition containing the said near-infrared absorber.
본 발명에 따른 근적외선 흡수제는 불화 구리를 사용하지 않아 제조과정에서 불화수소와 같은 유독가스가 발생하지 않으며, 제조 시 증류수와 알코올을 혼합 사용함으로써 입자의 응집을 막아 입자화를 용이하게 하는 효과가 있다. Since the near-infrared absorber according to the present invention does not use copper fluoride, toxic gases such as hydrogen fluoride are not generated during the manufacturing process, and the distilled water and alcohol are mixed during preparation to prevent the aggregation of particles, thereby facilitating granulation. .
또한, 네오디늄 또는 이터비움 화합물을 첨가함으로써 근적외선 흡수능력이 월등히 향상되어 잉크 제조시 잉크의 40%이상을 기존의 근적외선 흡수제로 사용해야했던 것을 20% 이하로 낮추는 효과가 있으며, 페인트로 제조하여 적용하는 경우 근적외선 흡수능력이 우수하여 자동차 또는 건물 내의 온도를 낮출 수 있어 에너지 절감에 기여할 수 있다.
In addition, by adding neodymium or ytterbium compounds, the near-infrared absorption ability is greatly improved, and it is effective to lower 40% or more of the ink used as a conventional near-infrared absorber to 20% or less when ink is manufactured. In this case, the near-infrared absorption ability is excellent, which can lower the temperature in the vehicle or building, thereby contributing to energy saving.
도 1은 근적외선 흡수제를 사용한 잉크의 광반사율 측정 결과를 나타낸 것이다. 1 shows light reflectance measurement results of an ink using a near infrared absorber.
본 발명에서는 네오디늄 또는 이터비움 화합물을 포함하여 구리계 근적외선 흡수제를 제조하는 경우 유독가스가 발생되지 않고 근적외선 흡수 능력이 향상된다는 것을 확인하고자 하였다. In the present invention, when preparing a copper-based near-infrared absorber including neodymium or iterium compound, it was confirmed that no toxic gas is generated and the near-infrared absorption ability is improved.
본 발명은 일 관점에서, 구리화합물; 인 화합물; 및 네오디늄 또는 이터비움 화합물로 이루어지는 것을 특징으로 하는 근적외선 흡수제에 관한 것이다. In one aspect, the present invention, a copper compound; Phosphorus compounds; And a near-infrared absorber comprising a neodymium or an etherium compound.
본 발명에서 근적외선은 700 내지 1300nm의 파장을 가지는 빛살을 말하며, 가시광선에 가깝지만 육안으로는 보이지 않는 비가시광 영역이다. In the present invention, near-infrared refers to light having a wavelength of 700 to 1300 nm, and is an invisible light region close to visible light but not visible to the naked eye.
본 발명에 있어서, 상기 구리화합물은 수산화구리(Cu(OH)2), 염화구리(CuCl2), 황산구리(CuSO4), 질산구리(Cu(NO3)2) 및 산화 구리(CuO)로 구성된 군에서 선택된 하나 이상인 것을 특징으로 할 수 있다. 이 구리화합물은 2가 구리 화합물인 것이 바람직하며, 인 화합물에 의해 용해되어 착화합물을 형성하고, 불화구리를 사용하지 않아 불화수소와 같은 유독가스가 발생하지 않는다. In the present invention, the copper compound is composed of copper hydroxide (Cu (OH) 2 ), copper chloride (CuCl 2 ), copper sulfate (CuSO 4 ), copper nitrate (Cu (NO 3 ) 2 ) and copper oxide (CuO) It may be characterized in that one or more selected from the group. It is preferable that this copper compound is a divalent copper compound, and it melt | dissolves with a phosphorus compound, and forms a complex compound, and copper fluoride is not used and no toxic gas, such as hydrogen fluoride, is generated.
본 발명에 있어서, 상기 인화합물은 인산(P2O5?nH2O의 총칭, 오르토인산, 메타인산 등을 포함함), 폴리인산((PnO3n +1)(n+2)-) 및 오산화인(P2O5)으로 구성된 군에서 선택된 하나 이상인 것을 특징으로 할 수 있다. 상기 언급한 바와 같이 인화합물은 구리화합물과 만나 착화합물을 형성한다.In the present invention, the phosphorus compound includes phosphoric acid (including P 2 O 5 ? NH 2 O generically, orthophosphoric acid, metaphosphoric acid, etc.), polyphosphoric acid ((P n O 3n +1 ) (n + 2)- ) And phosphorus pentoxide (P 2 O 5 ) may be at least one selected from the group consisting of. As mentioned above, the phosphorus compound meets with the copper compound to form a complex compound.
또한, 본 발명에 있어서, 상기 네오디늄 화합물은 산화네오디늄(Nd2O3), 염화네오디늄(NdCl3) 및 질산네오디늄(Nd(NO3)3)으로 구성된 군에서 선택된 하나 이상인 것을 특징으로 할 수 있으며, 상기 이터비움 화합물은 산화이터비움(Yb2O3), 염화이터비움(YbCl3) 및 질산이터비움(Yb(NO3)3)으로 구성된 군에서 선택된 하나 이상인 것을 특징으로 할 수 있다. 상기 네오디늄 또는 이터비움 화합물은 구리계 근적외선 흡수제에 포함되는 경우 근적외선 흡수능을 향상시킨다. In addition, in the present invention, the neodynium compound is at least one selected from the group consisting of neodymium oxide (Nd 2 O 3 ), neodymium chloride (NdCl 3 ) and neodymium nitrate (Nd (NO 3 ) 3 ). The iterium compound may be at least one selected from the group consisting of ytterbium oxide (Yb 2 O 3 ), ytterbium chloride (YbCl 3 ) and ytterbium nitrate (Yb (NO 3 ) 3 ). Can be. The neodymium or the iterium compound improves the near infrared absorption ability when included in the copper-based near infrared absorber.
본 발명에 따른 근적외선 흡수제는 바람직한 몰수 비로서, 상기 네오디늄 또는 이터비움 화합물의 함량이 상기 구리화합물의 0.01 내지 0.10 몰로 구성될 수 있다. 네오디늄 또는 이터비움 화합물의 함량이 구리화합물의 0.10 몰 이상이 되는 경우 근적외선 흡수능력이 더 이상 향상되지 않으며, 네오디늄 또는 이터비움 화합물이 구리화합물보다 고가이므로, 바람직하게는, 네오디늄 또는 이터비움 화합물의 함량이 구리화합물의 0.05 몰 이하로 구성될 수 있다. The near-infrared absorber according to the present invention is a preferred molar ratio, the content of the neodymium or etherium compound may be composed of 0.01 to 0.10 moles of the copper compound. When the content of neodymium or iterium compound is 0.10 mol or more of the copper compound, the near-infrared absorption capacity is no longer improved, and since neodynium or iterium compound is more expensive than the copper compound, preferably, neodymium or iterium The content of the compound may consist of 0.05 mole or less of the copper compound.
또한, 본 발명에 따른 근적외선 흡수제는 인화합물의 함량이 구리화합물의 0.5 내지 1.0 몰로 구성되는 것이 근적외선 흡수 능력을 향상시키기 위해서 바람직하다. In addition, the near-infrared absorber according to the present invention is preferably composed of 0.5 to 1.0 mole of the phosphorus compound in order to improve the near-infrared absorption ability.
본 발명은 다른 관점에서, 알코올 수용액에 구리화합물, 인화합물 및 네오디늄 또는 이터비움 화합물을 혼합하여 실온에서 교반, 여과 및 수세 후 건조시키는 단계; 상기 혼합물을 전기로에 넣어 서서히 가열하면서 소성하는 단계; 및 상기 소성된 혼합물을 해쇄기를 사용하여 입자화하는 단계를 포함하는 근적외선 흡수제의 제조방법에 관한 것이다. In another aspect, the present invention comprises the steps of mixing a copper compound, a phosphorus compound and a neodymium or etherium compound in an aqueous alcohol solution, followed by stirring, filtration and washing at room temperature, followed by drying; Sintering the mixture into an electric furnace and slowly heating it; And it relates to a method for producing a near infrared absorber comprising the step of granulating the calcined mixture using a crusher.
본 발명에 있어서, 상기 알코올 수용액은 구리계 근적외선 흡수제의 제조 공정에 포함되어, 형성된 입자의 응집을 방지하는 역할을 하는 것을 확인하였다. 기존의 물만 사용하여 구리계 근적외선 흡수제를 제조하는 기술에서는, 형성된 입자가 물에서 응집되어 입자화가 용이하지 않았지만, 본 발명에 따르면 알코올 수용액을 사용함으로써 형성된 입자가 응집되지 않도록 할 수 있다. 본 발명의 알코올 수용액의 농도는 25 내지 45 (v/v)인 것을 특징으로 할 수 있다. 알코올 수용액의 농도가 25 (v/v) 이하로 너무 낮으면, 근적외선 흡수제의 입자화가 잘 이루어지지 않고, 45 (v/v) 이상으로 너무 높으면 근적외선 흡수제의 제조 수욜이 낮아지는 문제가 발생한다. 본 발명에서 상기 알코올은 에탄올(ethanol), 메탄올(methanol), 이소프로필알코올(isopropyl alcohol) 및 부탄올(butanol)로 구성된 군에서 선택된 하나 이상인 것을 특징으로 할 수 있다. In the present invention, the aqueous alcohol solution was included in the manufacturing process of the copper-based near infrared absorber, it was confirmed that serves to prevent aggregation of the formed particles. In the conventional technique for producing a copper-based near-infrared absorber using only water, although the formed particles are agglomerated in water and not easily granulated, the present invention can prevent the formed particles from agglomerating by using an aqueous alcohol solution. The concentration of the aqueous alcohol solution of the present invention may be characterized in that 25 to 45 (v / v). If the concentration of the aqueous alcohol solution is too low below 25 (v / v), the near-infrared absorber is not granulated well, and if it is too high above 45 (v / v), there is a problem that the production of the near-infrared absorber is lowered. The alcohol in the present invention may be characterized in that at least one selected from the group consisting of ethanol (ethanol), methanol (methanol), isopropyl alcohol (isopropyl alcohol) and butanol (butanol).
본 발명에 있어서, 상기 소성 단계는 알루미나 도가니를 사용하는 것을 특징으로 할 수 있으며, 1 내지 2 시간 동안 200 내지 400℃까지 승온하고 약 1시간 유지 후 다시 700 내지 900℃까지 승온 후 1 내지 3 시간 유지 후 실온까지 냉각시키는 것을 특징으로 할 수 있다. In the present invention, the firing step may be characterized in that using an alumina crucible, and after the temperature is raised to 200 to 400 ℃ for 1 to 2 hours and maintained for about 1 hour and then again to 700 to 900 ℃ 1 to 3 hours It may be characterized by cooling to room temperature after the holding.
상기와 같이 제조된 근적외선 흡수제의 입자화는 해쇄기를 이용하여 분쇄하더라도 평균 약 2㎛ 정도의 미세한 입자가 얻어진다. 이 정도의 입자 크기는 요판 잉크, 그라비아 잉크, 평판 잉크, 스크린 잉크 등을 제조하기에 충분하다. In the granulation of the near-infrared absorber prepared as described above, fine particles having an average of about 2 μm can be obtained, even when pulverized using a crusher. This particle size is sufficient to produce intaglio inks, gravure inks, flat inks, screen inks and the like.
따라서, 본 발명은 다른 관점에서, 구리화합물, 인화합물 및 네오디늄 또는 이터비움 화합물을 포함하는 근적외선 흡수제를 포함하여 제조된 것을 특징으로 하는 잉크 조성물에 관한 것이다. Accordingly, the present invention relates to an ink composition, which is produced from another aspect, comprising a near-infrared absorber comprising a copper compound, a phosphorus compound and a neodymium or etherium compound.
본 발명에 따른 근적외선 흡수제는 잉크 제조용 바니시, 분산체, 용제 및 건조지연제와 혼합하고 연육함으로써 잉크로 제조할 수 있다. 상기 근적외선 흡수제에 있어서, 네오디늄 화합물을 포함하여 제조하는 경우 연녹색을 가지는 인쇄물이 얻어지고, 이터비움 화합물을 포함하여 제조하는 경우 청색을 가지는 인쇄물을 얻을 수 있다는 것을 확인하였다. The near-infrared absorbent according to the present invention can be prepared with ink by mixing and grinding with varnishes, dispersions, solvents and drying retardants for ink manufacture. In the near-infrared absorber, it was confirmed that a printed matter having a pale green color was obtained when the neodymium compound was prepared, and a printed matter having a blue color was obtained when the neodymium compound was produced.
본 발명에 따른 근적외선 흡수제를 포함하여 제조된 잉크 조성물은 근적외선을 흡수하는 능력이 뛰어나기 때문에, 보안 문서의 위조 또는 변조를 방지하기 위한 잉크로 활용할 수 있다. Since the ink composition prepared by using the near-infrared absorbent according to the present invention has an excellent ability to absorb near-infrared, it can be used as an ink for preventing forgery or tampering of a security document.
본 발명에 따른 근적외선 흡수 물질은 잉크 뿐만 아니라 페인트 조성물로 제조될 수 있다. 상기 페인트 조성물은 종래의 공지된 페인트 조성물에 본 발명에 따른 근적외선 흡수 물질을 첨가하는 것으로 제조될 수 있으며, 자동차용 기능성 페인트 조성물 또는 건축 내/외장제용 기능성 페인트 조성물로 활용되는 경우, 근적외선 흡수능력이 우수하여 자동차 또는 건물 내의 온도를 낮출 수 있어 에너지 절감에 기여할 수 있다.
The near-infrared absorbing material according to the present invention can be made with ink as well as paint compositions. The paint composition may be prepared by adding the near-infrared absorbing material according to the present invention to a conventionally known paint composition, and when used as a functional paint composition for automobiles or a functional paint composition for interior / exterior construction, the near-infrared absorbing ability may be reduced. It is excellent and can lower the temperature in the car or building, contributing to energy saving.
이하, 실시예를 통하여 본 발명을 더욱 상세히 설명하고자 한다. 이들 실시예는 오로지 본 발명을 예시하기 위한 것으로, 본 발명의 범위가 이들 실시예에 의해 제한되는 것으로 해석되지 않는 것은 당업계에서 통상의 지식을 가진 자에게 있어서 자명할 것이다.
Hereinafter, the present invention will be described in more detail with reference to Examples. It is to be understood by those skilled in the art that these embodiments are only for illustrating the present invention and that the scope of the present invention is not construed as being limited by these embodiments.
2ℓ 비이커에 물 400㎖와 에탄올 200㎖를 넣고 수산화구리 81g(0.75몰), 인산(85%) 60g(0.50몰), 산화네오디늄 10g(0.03몰)을 혼합하여 실온에서 4시간 교반한 다음 여과, 수세 후 오븐에서 105℃로 건조하였다. 상기 혼합물을 알루미나 도가니에 담아 전기로에 넣고 1시간에 걸쳐 300℃까지 올리고 1시간 유지 후 다시 800℃까지 올린 다음 2시간 유지한 후 실온까지 냉각시킨 결과, 연녹색 분말이 얻어졌다. 400 ml of water and 200 ml of ethanol were added to a 2 l beaker, followed by mixing 81 g (0.75 mol) of copper hydroxide, 60 g (0.50 mol) of phosphoric acid (85%), and 10 g (0.03 mol) of neodymium oxide, stirring at room temperature for 4 hours, and then filtering. After washing with water, it was dried in an oven at 105 ° C. The mixture was put in an alumina crucible, put in an electric furnace, heated to 300 ° C. over 1 hour, maintained at 800 ° C. for 2 hours, and then maintained for 2 hours, and cooled to room temperature. As a result, a pale green powder was obtained.
이를 미세 입자화하기 위해 로터밀(Roto-Mill)방식의 해쇄기(독일, FRITSCH사, Pulverizer-14)로 처리하였으며, 처리 조건은 17,000rpm/min으로 하였다.In order to finely granulate it, it was treated with a Roto-Mill crusher (Germany, FRITSCH, Pulverizer-14), and the treatment conditions were 17,000 rpm / min.
제조된 근적외선 흡수제의 입자는 입자분석기(영국, MALVERN사, MS-20)를 이용하여 측정한 결과 평균입자는 3㎛였다. The average particle size of the prepared near-infrared absorber was measured using a particle analyzer (MS-20, UK, MALVERN, Inc.).
제조된 근적외선 흡수제를 이용하여 바니시(NazDar S-227(미국 Nazdar Co. 제품)) 58 wt% , 분산제(Disperbyk-118(독일 BYK Chemie 제품)) 3 wt%, 용제(아농) 16 wt%, 건조지연제(동독류) 3 wt% 및 근적외선 흡수제 20 wt%의 조성으로 스크린잉크로 만들고 이를 사용하여 스크린인쇄 후 광반사율을 UV-VIS-NIR Spectrophotometer 5000(Varian사 제품)을 사용하여 측정한 결과를 도 1에 나타내었다.
58 wt% varnish (NazDar S-227 (manufactured by Nazdar Co.)), dispersant (Disperbyk-118 (manufactured by BYK Chemie)) 3 wt%, 16 wt% solvent (anon), dried using the prepared near infrared absorber The screen reflector was made with a composition of 3 wt% of a retardant (East poison) and 20 wt% of a near-infrared absorber and the light reflectance after screen printing was measured using a UV-VIS-NIR Spectrophotometer 5000 (Varian). 1 is shown.
2ℓ 비이커에 물 400㎖와 에탄올 200㎖를 넣고 수산화구리 79g(0.73몰), 인산(85%) 60g(0.50몰), 산화네오디늄 8.3g(0.025몰)을 혼합하여 실온에서 4시간 교반시킨 다음 여과, 수세 후 오븐에서 105℃로 건조하였다. 상기 혼합물을 알루미나 도가니에 담아 전기로에 넣고 1시간에 걸쳐 300℃까지 올리고 1시간 유지 후 다시 800℃까지 올린 다음 2시간 유지한 후 실온까지 냉각시킨 결과, 연녹색 분말이 얻어졌다. 400 ml of water and 200 ml of ethanol were added to a 2 l beaker, and 79 g (0.73 mol) of copper hydroxide, 60 g (0.50 mol) of phosphoric acid (85%) and 8.3 g (0.025 mol) of neodymium oxide were mixed and stirred at room temperature for 4 hours. After filtration and washing with water, the resultant was dried at 105 ° C. in an oven. The mixture was put in an alumina crucible, put in an electric furnace, heated to 300 ° C. over 1 hour, maintained at 800 ° C. for 2 hours, and then held for 2 hours, and cooled to room temperature. A light green powder was obtained.
이를 미세 입자화하기 위해 로터밀(Roto-Mill)방식의 해쇄기(독일, FRITSCH사, Pulverizer-14)로 처리하였으며, 처리 조건은 17,000rpm/min으로 하였다.In order to finely granulate it, it was treated with a Roto-Mill crusher (Germany, FRITSCH, Pulverizer-14), and the treatment conditions were 17,000 rpm / min.
제조된 근적외선 흡수제의 입자는 입자분석기(영국, MALVERN사, MS-20)를 이용하여 측정한 결과 평균입자는 3㎛이었다. The average particle size of the prepared near-infrared absorber was measured using a particle analyzer (MS-20, MALVERN, UK).
제조된 근적외선 흡수제를 이용하여 바니시(NazDar S-227(미국 Nazdar Co. 제품)) 58 wt%, 분산제(Disperbyk-118(독일 BYK Chemie 제품)) 3 wt%, 용제(아농) 16 wt%, 건조지연제(동독류) 3 wt% 및 근적외선 흡수제 20 wt%의 조성으로 스크린잉크로 만들고 이를 사용하여 스크린인쇄 후 광반사율을 UV-VIS-NIR Spectrophotometer 5000(Varian사 제품)을 사용하여 측정한 결과를 도 1에 나타내었다.
58 wt% varnish (NazDar S-227 (manufactured by Nazdar Co.)), 3 wt% dispersant (Disperbyk-118 (manufactured by BYK Chemie, Germany)), 16 wt% solvent (Anon), and dried using the prepared near infrared absorber The screen reflector was made with a composition of 3 wt% of a retardant (East poison) and 20 wt% of a near-infrared absorber and the light reflectance after screen printing was measured using a UV-VIS-NIR Spectrophotometer 5000 (Varian). 1 is shown.
2ℓ 비이커에 물 400㎖와 에탄올 200㎖를 넣고 산화구리 79.4g(0.99몰), 인산(85%) 77g(0.67몰), 산화이터비움 3.94g(0.01몰)을 혼합하여 실온에서 4시간 교반시킨 다음 여과, 수세 후 오븐에서 105℃로 건조하였다. 상기 혼합물을 알루미나 도가니에 담아 전기로에 넣고 1시간에 걸쳐 300℃까지 올리고 1시간 유지 후 다시 800℃까지 올린 다음 2시간 유지한 후 실온까지 냉각시킨 결과, 청색 분말이 얻어졌다.400 ml of water and 200 ml of ethanol were added to a 2-liter beaker. Copper oxide 79.4 g (0.99 mol), phosphoric acid (85%) 77 g (0.67 mol), and ether oxide 3.94 g (0.01 mol) were mixed and stirred at room temperature for 4 hours. Then filtered and washed with water and dried in an oven at 105 ℃. The mixture was put in an alumina crucible, put in an electric furnace, heated to 300 ° C. over 1 hour, maintained at 800 ° C. for 2 hours, and then maintained for 2 hours, and cooled to room temperature. A blue powder was obtained.
이를 미세 입자화하기 위해 로터밀(Roto-Mill)방식의 해쇄기(독일, FRITSCH사, Pulverizer-14)로 처리하였으며, 처리 조건은 17,000rpm/min으로 하였다.In order to finely granulate it, it was treated with a Roto-Mill crusher (Germany, FRITSCH, Pulverizer-14), and the treatment conditions were 17,000 rpm / min.
제조된 근적외선 흡수제의 입자는 입자분석기(영국, MALVERN사, MS-20)를 이용하여 측정한 결과 평균입자는 3㎛이었다. The average particle size of the prepared near-infrared absorber was measured using a particle analyzer (MS-20, MALVERN, UK).
제조된 근적외선 흡수제를 이용하여 바니시(NazDar S-227(미국 Nazdar Co. 제품)) 58 wt%, 분산제(Disperbyk-118(독일 BYK Chemie 제품)) 3 wt%, 용제(아농) 16 wt%, 건조지연제(동독류) 3 wt% 및 근적외선 흡수제 20 wt%의 조성으로 스크린잉크로 만들고 이를 사용하여 스크린인쇄 후 광반사율을 UV-VIS-NIR Spectrophotometer 5000(Varian사 제품)을 사용하여 측정한 결과를 도 1에 나타내었다.
58 wt% varnish (NazDar S-227 (manufactured by Nazdar Co.)), 3 wt% dispersant (Disperbyk-118 (manufactured by BYK Chemie, Germany)), 16 wt% solvent (Anon), and dried using the prepared near infrared absorber The screen reflector was made with a composition of 3 wt% of a retardant (East poison) and 20 wt% of a near-infrared absorber and the light reflectance after screen printing was measured using a UV-VIS-NIR Spectrophotometer 5000 (Varian). 1 is shown.
비교예Comparative example
1 One
대한민국등록특허공보 제10-0618083호의 명세서에 개시된 실시예 1과 같이, 2 ℓ 비이커에 물 500㎖를 넣고 수산화구리 70g, 인산(85%) 90g, 붕산 80g, 산화알루미늄 5g, 플루오르붕산 150g을 혼합하여 고화한 다음 고화물을 전기로에 넣어 950℃로 소성하고 실온까지 냉각하였다. As in Example 1 disclosed in the specification of Korean Patent Publication No. 10-0618083, 500 ml of water was added to a 2 l beaker, and 70 g of copper hydroxide, 90 g of phosphoric acid (85%), 80 g of boric acid, 5 g of aluminum oxide, and 150 g of fluoroboric acid were mixed. The solidified product was put into an electric furnace, calcined at 950 ° C., and cooled to room temperature.
이 소성물은 백색이고 미세입자가 뭉쳐있는 발포형 상태이므로 미세 입자화하기 위해 로터밀(Roto-Mill)방식의 해쇄기(독일, FRITSCH사, Pulverizer-14)로 처리하였으며, 처리 조건은 17,000rpm/min으로 하였다.This fired product was white and foamed state in which fine particles were agglomerated, so it was treated with a Roto-Mill crusher (Pulverizer-14, FRITSCH, Germany) to make fine particles. It was / min.
제조된 근적외선 흡수제의 입자는 입자분석기(영국, MALVERN사, MS-20)를 이용하여 측정한 결과 평균입자는 3㎛이었다. The average particle size of the prepared near-infrared absorber was measured using a particle analyzer (MS-20, MALVERN, UK).
제조된 근적외선 흡수제를 이용하여 바니시(NazDar S-227(미국 Nazdar Co. 제품)) 42 wt%, 분산제(Disperbyk-118(독일 BYK Chemie 제품)) 3 wt%, 용제(아농) 12 wt%, 건조지연제(동독류) 3 wt% 및 근적외선 흡수제 40 wt%의 조성으로 스크린잉크로 만들고 이를 사용하여 스크린인쇄 후 광반사율을 UV-VIS-NIR Spectrophotometer 5000(Varian사 제품)을 사용하여 측정한 결과를 도 1에 나타내었다.
Varnish (NazDar S-227 (manufactured by Nazdar Co.)) 42 wt%, Dispersant (Disperbyk-118 (manufactured by BYK Chemie)) 3 wt%, Solvent (anon) 12 wt%, using the prepared near infrared absorber The screen reflector was made with a composition of 3 wt% of a retardant (East poison) and 40 wt% of a near-infrared absorber, and the light reflectance after screen printing was measured using a UV-VIS-NIR Spectrophotometer 5000 (Varian). 1 is shown.
도 1은 실시예 1 내지 3 및 비교예에 따른 근적외선 흡수제를 사용한 잉크의 광반사율(%R)을 나타낸 것이다. 4가지 예에서 모두 700~1300nm의 파장범위를 흡수하고 있는 것을 확인할 수 있다. 종래의 기술에 따른 근적외선 흡수제를 40% 함유하는 잉크(비교예 1)의 광반사율은 800~1000nm 파장에서 약 10% 정도로 약 90%의 근적외선을 흡수하는 능력을 나타내었다. 본 발명에 따른 근적외선 흡수제를 20% 함유하는 잉크(실시예 1 내지 3)의 광반사율은 실시예 1 의 경우 40%를 함유하고 있는 비교예 1보다 더 낮은 반사율을 나타내었으며, 실시예 2의 경우 거의 유사, 실시예 3의 경우 25% 정도의 광반사율을 나타내었다. 종래의 잉크 제조 기술에서, 안료의 함량이 반으로 줄어드는 경우 광반사율이 4배 가량 증가되는 것과 비교하면 본 발명의 실시예에서 월등히 뛰어난 근적외선 흡수능을 보이는 것을 알 수 있다. 1 shows light reflectance (% R) of an ink using a near infrared absorber according to Examples 1 to 3 and Comparative Examples. In all four examples, it can be seen that the wavelength range of 700 to 1300 nm is absorbed. The light reflectance of the ink (Comparative Example 1) containing 40% of the near-infrared absorber according to the prior art showed the ability to absorb about 90% of the near-infrared at about 10% at the wavelength of 800-1000 nm. The light reflectance of the ink (Examples 1 to 3) containing 20% of the near-infrared absorbent according to the present invention showed a lower reflectance than Comparative Example 1 containing 40% in Example 1, and in Example 2 Almost similarly, Example 3 showed about 25% light reflectance. In the conventional ink manufacturing technology, when the content of the pigment is reduced by half, it can be seen that the near-infrared absorbing ability is excellent in the embodiment of the present invention as compared with the increase in the light reflectance by about 4 times.
즉, 본 발명에 따른 근적외선 흡수제를 20%만 함유하도록 잉크를 제조하여도, 종래 기술에 의한 근적외선 흡수제를 40% 함유한 잉크보다 뛰어나거나 유사한 광흡수율을 나타낸 것을 확인할 수 있었으며, 따라서, 본 발명에 따른 근적외선 흡수제의 근적외선 흡수능이 종래의 기술에 따른 근적외선 흡수제보다 월등히 뛰어난 것을 확인하였다.
That is, even when the ink was prepared to contain only 20% of the near-infrared absorbent according to the present invention, it was confirmed that the ink showed superior or similar light absorption rate to the ink containing 40% of the near-infrared absorber according to the prior art. It was confirmed that the near-infrared absorbing ability of the near-infrared absorbent was much superior to the near-infrared absorbent according to the prior art.
이상으로 본 발명 내용의 특정한 부분을 상세히 기술하였는 바, 당업계의 통상의 지식을 가진 자에게 있어서 이러한 구체적 기술은 단지 바람직한 실시태양일 뿐이며, 이에 의해 본 발명의 범위가 제한되는 것이 아닌 점을 명백할 것이다. 따라서, 본 발명의 실질적인 범위는 첨부된 청구항들과 그것들의 등가물에 의하여 정의된다고 할 것이다.
Having described the specific part of the present invention in detail, it is apparent to those skilled in the art that such a specific technology is only a preferred embodiment, thereby not limiting the scope of the present invention. something to do. Thus, the substantial scope of the present invention will be defined by the appended claims and their equivalents.
Claims (15)
Copper compounds; Phosphorus compounds; And a near-infrared absorber comprising neodymium or iterium compounds.
The near-infrared absorber of claim 1, wherein the wavelength of the near infrared ray is 700 to 1300 nm.
The near-infrared absorber of claim 1, wherein the copper compound is at least one selected from the group consisting of copper hydroxide, copper chloride, copper sulfate, copper nitrate, and copper oxide.
The near-infrared absorber of claim 1, wherein the phosphorus compound is at least one selected from the group consisting of phosphoric acid, polyphosphoric acid, and phosphorus pentoxide.
The near-infrared absorber of claim 1, wherein the neodynium compound is at least one selected from the group consisting of neodymium oxide, neodymium chloride, and neodymium nitrate.
The near-infrared absorbent of claim 1, wherein the iterium compound is at least one selected from the group consisting of ytterbium oxide, ytterbium chloride, and yterbium nitrate.
The near-infrared absorber according to claim 1, wherein the content of neodymium or iterium oxide is 0.01 to 0.10 moles of the copper compound.
The near-infrared absorber according to claim 1, wherein the content of the phosphorus compound is 0.5 to 1.0 mole of the copper compound.
상기 혼합물을 전기로에 넣어 서서히 가열하면서 소성하는 단계; 및
상기 소성된 혼합물을 분쇄하여 입자화하는 단계를 포함하는 근적외선 흡수제의 제조방법.
Mixing a copper compound, a phosphorus compound and a neodymium or etherium compound in an aqueous alcohol solution, followed by stirring, filtration and washing at room temperature, followed by drying;
Sintering the mixture into an electric furnace and slowly heating it; And
Method for producing a near-infrared absorber comprising the step of pulverizing the calcined mixture.
10. The method of claim 9, wherein the concentration of the aqueous alcohol solution is 25 to 45 (v / v).
The method of claim 9, wherein the alcohol is at least one selected from the group consisting of ethanol, methanol, isopropyl alcohol and butanol.
10. The method of claim 9, wherein the firing step uses an alumina crucible.
10. The method of claim 9, wherein the firing step is to increase the temperature to 200 to 400 ℃ for 1 to 2 hours, after maintaining for about 1 hour and then again to 700 to 900 ℃ after maintaining for 1 to 3 hours and then cooled to room temperature Method for preparing absorbent.
An ink composition comprising the near infrared absorber of any one of claims 1 to 8.
The paint composition containing the near-infrared absorber of any one of Claims 1-8.
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| KR101717907B1 (en) * | 2016-03-29 | 2017-04-04 | 부성폴리콤 주식회사 | Near-infrared absorption white material and its manufacturing method |
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| KR101717907B1 (en) * | 2016-03-29 | 2017-04-04 | 부성폴리콤 주식회사 | Near-infrared absorption white material and its manufacturing method |
| WO2017171342A3 (en) * | 2016-03-29 | 2018-08-02 | 부성폴리콤 주식회사 | Near-infrared absorbing white material and preparation method thereof |
| US10926354B2 (en) | 2016-03-29 | 2021-02-23 | Buseong Polycom Co., Ltd. | Near-infrared absorbing white material and preparation method thereof |
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