JP7320691B1 - Cu-Cr-Zn-O複合酸化物顔料 - Google Patents
Cu-Cr-Zn-O複合酸化物顔料 Download PDFInfo
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- JP7320691B1 JP7320691B1 JP2023523268A JP2023523268A JP7320691B1 JP 7320691 B1 JP7320691 B1 JP 7320691B1 JP 2023523268 A JP2023523268 A JP 2023523268A JP 2023523268 A JP2023523268 A JP 2023523268A JP 7320691 B1 JP7320691 B1 JP 7320691B1
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- pigment
- composite oxide
- oxide
- oxide pigment
- glass
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- 239000000049 pigment Substances 0.000 title claims abstract description 222
- 239000002131 composite material Substances 0.000 title claims abstract description 111
- 229910007541 Zn O Inorganic materials 0.000 title claims abstract description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000000203 mixture Substances 0.000 claims abstract description 27
- 239000011787 zinc oxide Substances 0.000 claims abstract description 24
- 239000011701 zinc Substances 0.000 claims abstract description 18
- 229910016462 cZnO Inorganic materials 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 30
- 239000011521 glass Substances 0.000 claims description 29
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 claims description 18
- 238000002845 discoloration Methods 0.000 claims description 15
- 238000002441 X-ray diffraction Methods 0.000 claims description 14
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- 239000003973 paint Substances 0.000 claims description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 9
- 238000004040 coloring Methods 0.000 claims description 5
- 150000001845 chromium compounds Chemical class 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
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- 239000007858 starting material Substances 0.000 claims description 3
- 150000003752 zinc compounds Chemical class 0.000 claims description 3
- 239000005749 Copper compound Substances 0.000 claims description 2
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- 150000001880 copper compounds Chemical class 0.000 claims description 2
- 230000000052 comparative effect Effects 0.000 description 40
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 21
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 8
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- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 6
- 229910000423 chromium oxide Inorganic materials 0.000 description 6
- 229910000431 copper oxide Inorganic materials 0.000 description 6
- 239000006104 solid solution Substances 0.000 description 6
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
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- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 4
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- 238000002360 preparation method Methods 0.000 description 4
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- 229910052721 tungsten Inorganic materials 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 229910017813 Cu—Cr Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- 229910052726 zirconium Inorganic materials 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
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- 229910016510 CuCrO2 Inorganic materials 0.000 description 1
- KSPIHGBHKVISFI-UHFFFAOYSA-N Diphenylcarbazide Chemical compound C=1C=CC=CC=1NNC(=O)NNC1=CC=CC=C1 KSPIHGBHKVISFI-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- MZZSDCJQCLYLLL-UHFFFAOYSA-N Secalonsaeure A Natural products COC(=O)C12OC3C(CC1=C(O)CC(C)C2O)C(=CC=C3c4ccc(O)c5C(=O)C6=C(O)CC(C)C(O)C6(Oc45)C(=O)OC)O MZZSDCJQCLYLLL-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- GXDVEXJTVGRLNW-UHFFFAOYSA-N [Cr].[Cu] Chemical compound [Cr].[Cu] GXDVEXJTVGRLNW-UHFFFAOYSA-N 0.000 description 1
- RHQKKJPJCHGKQO-UHFFFAOYSA-N [Cu+2].[O-][Cr]([O-])=O Chemical class [Cu+2].[O-][Cr]([O-])=O RHQKKJPJCHGKQO-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 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
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- 238000007796 conventional method Methods 0.000 description 1
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- JGDFBJMWFLXCLJ-UHFFFAOYSA-N copper chromite Chemical compound [Cu]=O.[Cu]=O.O=[Cr]O[Cr]=O JGDFBJMWFLXCLJ-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- 150000004679 hydroxides Chemical class 0.000 description 1
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- 150000002506 iron compounds Chemical class 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(iii) oxide Chemical compound O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 238000005375 photometry Methods 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- DNYWZCXLKNTFFI-UHFFFAOYSA-N uranium Chemical compound [U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U][U] DNYWZCXLKNTFFI-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
技術・染色技術協会(The American Association of Textile Chemists and Colorists:AATTC)によって規定されたカラーインデックスに登録されている複合酸化物顔料C.I.ピグメントブラック28は、CuおよびCrからなるスピネル構造を有する青みの黒顔料であり、耐薬品性、耐熱性、および耐候性に優れた非常に堅牢度の高い顔料である。
下させることができる複合酸化物顔料が記述されている。しかし、顔料の耐久性については記述されていない。また、本願出願人が後に詳細に説明するように、特許文献3に開示されている組成物では、十分な高温安定性が保証されているものではない。
酸化物の組成式:aCuO・bCr2O3・cZnO(mol%)を有し、式中、0.1≦c≦5、45≦a+c≦55、45≦b≦55(a+b+c=100)である、Cu-Cr-Zn-O複合酸化物顔料に関するものである。
式AaCubMncCrdO4を有する亜クロム酸銅系固溶体を含み、
Aは、Al、Mg、Ti、Fe、Co、Ni、Zn、Zr、Nb、Y、W、Sb、及びCaからなる群から選択される少なくとも1つの金属であり、
2.6≦a+b+c+d≦3.2であり、
a、b、及びdのいずれも零ではない、改変亜クロム酸銅黒色スピネルが開示されている。
1.引用文献1は、その段落[0017]に記載されているように、「低下したCTEを有する黒色顔料を得る」ことを課題としたものであり、その課題を解決するために、「Al、Mg、Ti、Fe、Co、Ni、Zn、Zr、Nb、Y、W、Sb、及びCaからなる群から選択される少なくとも1つの金属」である二次改変剤を採用しようとしたものである。
2.本願発明におけるCu-Cr-Zn-O複合酸化物顔料は、スピネル構造CuCr2O4を有するCu-Cr-O複合酸化物に、修飾酸化物として添加した酸化亜鉛由来のZnが固溶してなるものである。
次に本発明を具体的に説明するために、本発明の実施例およびこれとの比較を示す為の比較例をいくつか挙げる。
以下の実施例1~21において、組成式aCuO・bCr2O3・cZnO(mol%)に基づき、0.1≦c≦10、かつ40≦a+b≦60、かつ40≦b≦60(a+b+c=100)を満たすような範囲で(a、b、c)を種々変更して目的とする顔料組成となるように酸化銅、酸化クロム、酸化亜鉛を総重量100gになるよう所定量秤量した。(a、b、c)の具体的な値は、下記の表1に示した。
実施例1~21とは異なり、aCuO・bCr2O3(mol%)に基づき、45≦a≦55、かつ45≦b≦55(a+b=100)の範囲で(a、b)を選び、修飾酸化物を含まないCuおよびCrからなるCu-Cr-O複合酸化物顔料を作製した。
aCuO・bCr2O3・cMn2O3(mol%)に基づき、45≦a≦55、かつ40≦b≦50、かつc=5(a+b+c=100)の範囲で(a、b、c)とし、従来から修飾酸化物として添加される二酸化マンガンMnO2由来の金属元素Mn含むCu、Cr、およびMnからなるCu-Cr-Mn-O複合酸化物顔料を作製した。
aCuO・bCr2O3・cFe2O3(mol%)に基づき、45≦a≦55、かつ40≦b≦50、かつc=5(a+b+c=100)の範囲で(a、b、c)を選び、従来から修飾酸化物として添加される酸化鉄Fe2O3由来の金属元素Feを含むCu、Cr、およびFeからなるCu-Cr-Fe-O複合酸化物顔料を、上記の実施例1~21
と同様の操作により作製した。
((a)色調)
アクリル樹脂100重量部に対して、実施例1~21および比較例1~9で得た複合酸化物顔料各10重量部を、ペイントコンディショナーにより分散させた。
実施例1~21および比較例1~9でそれぞれ作製したCu-Cr-Zn-O、Cu-Cr-O、Cu-Cr-Mn-O、あるいはCu-Cr-Fe-O複合酸化物顔料の中からそれぞれ最も色彩特性が優れていた組成を選定し、各々の成分系について焼成温度800℃、900℃、および1000℃で作製した顔料のXRD回折パターンを比較することで、顔料を作製する際の焼成温度の上昇に伴う顔料の結晶構造の変化を観察した。
(a)および(b)の評価結果より、作製したCu-Cr-Zn-O、Cu-Cr、Cu-Cr-Mn-O、あるいはCu-Cr-Fe-O複合酸化物顔料の中からそれぞれ最も色彩特性が優れ、且つ結晶構造に異相CuCrO2が検出されなかった組成を選定した。具体的には、実施例10の1000℃で焼成したCu-Cr-Zn-O複合酸化物顔料、比較例2の800℃で焼成したCu-Cr-O複合酸化物顔料、比較例5の800℃で焼成したCu-Cr-Mn-O複合酸化物顔料、および比較例8の800℃で焼成したCu-Cr-Fe-O複合酸化物顔料を選定した。
EPA3060A(ALKALINE DIGESTION FOR HEXAVALENT CHROMIUM) に基づく方法で、
実施例10の1000℃で焼成したCu-Cr-Zn-O複合酸化物顔料、比較例2の800℃で焼成したCu-Cr-O複合酸化物顔料、比較例5の800℃で焼成したCu-Cr-Mn-O複合酸化物顔料、および比較例8の800℃で焼成したCu-Cr-Fe-O複合酸化物顔料からの六価クロムの溶出液を作製した。溶出液中の六価クロム濃度をジフェニルカルバジド吸光光度法により測定した。(JISK0102)。
実施例10の1000℃で焼成したCu-Cr-Zn-O複合酸化物顔料、比較例2の800℃で焼成したCu-Cr-O複合酸化物顔料、比較例5の800℃で焼成したCu-Cr-Mn-O複合酸化物顔料、および比較例8の800℃で焼成したCu-Cr-Fe-O複合酸化物顔料について、顔料1.2g、およびビヒクル0.6gとなるように秤量し、フーバーマーラーを用いて十分に混合しペーストを作製した。作製したペーストは板ガラスの錫面に厚み76.2μmのアプリケータも用いて展色し、120℃の乾燥炉で30分間乾燥させた。さらに、この板ガラスを680℃の電気炉で20分間焼成を行い、十分に自然冷却させた後に板ガラス上の顔料を水道水で洗い流し、板ガラスの錫面における赤変の発現具合を観察した。
製した顔料のL*は12.0~16.2とすべての比較例において焼成温度の上昇に伴い
黒度は低下する傾向が観測された。
Claims (7)
- Cu-Cr-O複合酸化物に修飾酸化物として添加した酸化亜鉛由来のZnが固溶してなるCu-Cr-Zn-O複合酸化物顔料であって、
酸化物の組成式:aCuO・bCr2O3・cZnO(mol%)を有し、式中、0.1≦c≦5、45≦a+c≦55、45≦b≦55(a+b+c=100)である、Cu-Cr-Zn-O複合酸化物顔料。 - X線回折パターン中に、副生成物CuCrO2を含まないことを特徴とする請求項1に
記載のCu-Cr-Zn-O複合酸化物顔料。 - 銅化合物、クロム化合物、および亜鉛化合物を出発原料とし、乾式法によって混合したバッチを800~1000℃の温度で焼成すること特徴とし、スピネル構造が形成されたものである、請求項1に記載のCu-Cr-Zn-O複合酸化物顔料。
- 塗料、プラスチック、およびガラスの着色顔料として使用される、請求項1に記載のCu-Cr-Zn-O複合酸化物顔料。
- EPA3060A法に基づく顔料溶出液中の6価クロム溶出量が250ppm以下である、請求項1に記載のCu-Cr-Zn-O複合酸化物顔料。
- グラスカラーに使用され、フロート板ガラスの錫面に500~700℃で焼き付けた際に赤変が発現しない、請求項1に記載のCu-Cr-Zn-O複合酸化物顔料。
- Laser Direct Structuring(LDS)に使用される、請求項1に記載のCu-Cr-Zn-O複合酸化物顔料。
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