TW200706604A - Process for the production of pigment composition, colored composition for color filter obtained by said process, and color filter - Google Patents

Process for the production of pigment composition, colored composition for color filter obtained by said process, and color filter Download PDF

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Publication number
TW200706604A
TW200706604A TW95114255A TW95114255A TW200706604A TW 200706604 A TW200706604 A TW 200706604A TW 95114255 A TW95114255 A TW 95114255A TW 95114255 A TW95114255 A TW 95114255A TW 200706604 A TW200706604 A TW 200706604A
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Taiwan
Prior art keywords
pigment
composition
water
resin
derivative
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TW95114255A
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Chinese (zh)
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TWI462975B (en
Inventor
Takami Mori
Nobuyuki Segawa
Takuya Kotani
Hiroyuki Nakamura
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Toyo Ink Mfg Co
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Priority claimed from JP2005124620A external-priority patent/JP2006299138A/en
Priority claimed from JP2005131178A external-priority patent/JP2006306996A/en
Priority claimed from JP2006065683A external-priority patent/JP2007241050A/en
Application filed by Toyo Ink Mfg Co filed Critical Toyo Ink Mfg Co
Publication of TW200706604A publication Critical patent/TW200706604A/en
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Publication of TWI462975B publication Critical patent/TWI462975B/en

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D17/00Pigment pastes, e.g. for mixing in paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D17/00Pigment pastes, e.g. for mixing in paints
    • C09D17/003Pigment pastes, e.g. for mixing in paints containing an organic pigment
    • GPHYSICS
    • G02OPTICS
    • G02FOPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
    • G02F1/00Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
    • G02F1/01Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour 
    • G02F1/13Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour  based on liquid crystals, e.g. single liquid crystal display cells
    • G02F1/133Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
    • G02F1/1333Constructional arrangements; Manufacturing methods
    • G02F1/1335Structural association of cells with optical devices, e.g. polarisers or reflectors
    • G02F1/133509Filters, e.g. light shielding masks
    • G02F1/133514Colour filters

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Nonlinear Science (AREA)
  • Mathematical Physics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Optical Filters (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)

Description

200706604 九、發明說明: 【發明所屬之技術領域】 本發明涉及一種在載色劑中具有非常優異的分散性的 顏料組成物之製法,其中用於顯色的顆粒的粒子尺寸微細 而且粒子直徑均勻,並且涉及一種使用上述顏料組成物的 用=濾色器的著色組成物以及使用上述著色組成物的遽 色°°特別地,本發明涉及一種顏料組成物的製法,當它 用於顯色的粉末粒子分散在油墨、比如凹印油墨或膠印油 墨或塗料的載色劑中時’該顏料組成物提供了具有良好光 ,度=高著色強度的塗覆品。本發明還涉及一種用於濾色 器的著色組成物’其用於製備用在彩色液晶顯示器和彩色 攝像管元件中的據色器,本發明還涉及一種使用上述著色 組成物形成的滤色器。 【先前技術】 有些有機顏料,如偶氮顏料,其合成時選擇適當的反應 條件可=到微細和均勻的粒子。對於其他有機顏料如多^ 化銅酞月顏料而5,其在合成中產生的極細和成塊粒子可 =後處料增加和均自化。對於其他錢 進行稱作著色的處理’其在合成中產生的“ 和不均勻粒子的尺寸在後處理時被細碎和均句化。 右:ΐ二t青顏料具有漂亮的色彩和高著色強度而且具 有u各種性質如耐純和耐熱性 大 量用於著色材料工業領域。 匕称乏地大 通常,銅酞青顏料倍為登兩 丁十係在㊉壓或增壓下以及存在或缺少催 312XP/發明說明書(補件)/95-08/95114255 ^ 200706604 化劑如鉬酸銨或四氯化鈦的情況下,經酞酐或其衍生物、 尿素和銅源之間的反應、或者苯二甲腈 • (Phthalodinitrile)或其衍生物和有機溶劑如烷基苯、三 u 氯苯或硝基苯中的銅源之間的反應製備。 然而,合成的酞青分子在其合成溶劑中經由連續粒子生 長,以致於只獲得長軸直徑約為1〇到2〇〇//m的粗粒和針 狀粒子。因此,作為用於油墨、塗料、塑膠等的著色顏料, _其價值是非常低的,而且這種酞青被稱作粗銅酞青。因 此,需要微細地粉碎粗銅酞青以獲得在著色上具有高有效 性的粒子,即,具有約0·01到〇 5//m粒徑的粒子。 作為用於細碎粗銅酞青的工業方法,多種方法是已知 的。例如,已知所謂的溶劑鹽研磨方法(見Jp—A-7 —53889 和JP-A-5-43704),其中將少量的溶劑如二伸乙甘醇添加 到粗銅酞青和氯化鈉的混合物中,並且通過用球磨機、磨 碎機或分批揑合機將其劇烈揑合以濕磨由此潤濕的混合 籲物。在該方法中,經由用水洗滌以從揑合的混合物中去除 氯化鈉和二伸乙甘醇,並且接著乾燥,以獲得具有微細原 始粒子的銅敝青顏料。 而,t知的分批揑合機存在一些問題,比如由於它們 —的分批形式而限制了生產規模、批次之間質量變化、由於 -它們的開放式結構而混入雜質、卩及由於產生粉塵而污染 工作%境。此外,需要大量的能量用於細碎有機顏料,而 且在細碎水平上亦存在限制。此外,當將獲得的銅欧青顏 料分散在印刷油墨比如凹印油墨或膠印油墨或者塗料的 312XP/發明說明書(補件)/95-08/95114255 200706604 載色劑中並且使用獲得的銅酞青顏料時,總是需要改進它 的塗覆品的光澤度和著色強度。 在液晶顯示器中,夾在兩個偏光板之間的液晶層會控制 透過第一個偏光板的偏光角並且控制透過第二個偏光板 的光量,由此進行顯示。主要的液晶顯示器裝置是使用扭 曲向列(TN)型液晶的顯示器。經由在兩個偏光板之間提供 濾色裔使液晶顯示器能夠進行色彩顯示。最近幾年中,液 曰曰顯示為裝置被用在電視機和用於個人電腦的監視器 中。因為這個原因,愈加需要具有高亮度和高對比度的濾BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a process for producing a pigment composition having very excellent dispersibility in a vehicle, wherein particles for color development have fine particle sizes and uniform particle diameters. And relates to a coloring composition using a color filter using the above pigment composition and a tinge color using the above coloring composition. In particular, the present invention relates to a method for preparing a pigment composition, which is used for color development. When the powder particles are dispersed in an ink such as a gravure ink or an offset ink or a vehicle of a coating, the pigment composition provides a coating having good light, degree = high color strength. The present invention also relates to a coloring composition for a color filter for preparing a color filter for use in a color liquid crystal display and a color image pickup tube element, and to a color filter formed using the above colored composition . [Prior Art] Some organic pigments, such as azo pigments, are synthesized by selecting appropriate reaction conditions to fine and uniform particles. For other organic pigments such as copper cerium pigment 5, the extremely fine and agglomerated particles produced in the synthesis can be increased and self-automated. For other money, a process called coloring, which is produced in the synthesis, and the size of the uneven particles are finely divided and homogenized at the time of post-processing. Right: ΐ2t green pigment has beautiful color and high color strength and It has a variety of properties such as resistance to purity and heat resistance and is used in the industrial field of coloring materials. Nicknames are generally large, and copper phthalocyanine pigments are doubled under ten pressures or supercharged, and there is or lacks 312XP/ SUMMARY OF THE INVENTION (Supplement) /95-08/95114255 ^ 200706604 In the case of a reagent such as ammonium molybdate or titanium tetrachloride, a reaction between phthalic anhydride or a derivative thereof, a source of urea and copper, or a phthalonitrile • Preparation of a reaction between (Phthalodinitrile) or a derivative thereof and an organic solvent such as an alkylbenzene, tri-chlorobenzene or a copper source in nitrobenzene. However, the synthesized indigo molecule is grown by continuous particles in its synthetic solvent. Therefore, only coarse particles and acicular particles having a major axis diameter of about 1 〇 to 2 〇〇//m are obtained. Therefore, as a coloring pigment for inks, paints, plastics, etc., the value is very low. And this indigo is called blister copper. Therefore, it is necessary to finely pulverize the crude copper indigo to obtain particles having high effectiveness in coloring, that is, particles having a particle diameter of about 0·01 to 〇5//m. As an industry for finely crushed crude copper indigo Methods, various methods are known. For example, a so-called solvent salt grinding method is known (see Jp-A-7-53889 and JP-A-5-43704) in which a small amount of a solvent such as diethylene glycol is added. To a mixture of blister copper indigo and sodium chloride, and vigorously kneading it by a ball mill, an attritor or a batch kneader to wet-grind the thus mixed mixture. In this method, it is washed with water. Sodium chloride and diethylene glycol are removed from the kneaded mixture, and then dried to obtain a copper indigo pigment having fine primary particles. However, there are some problems with the batch kneader, such as due to them. The batch form limits the scale of production, the quality changes between batches, the incorporation of impurities due to their open structure, the contamination of the work due to the generation of dust, and the need for large amounts of energy for finely divided organic pigments. and There is also a limit on the level of fine crushing. In addition, when the obtained copper eucalyptus pigment is dispersed in a printing ink such as gravure ink or offset ink or paint, 312XP/invention specification (supplement)/95-08/95114255 200706604 In the agent and using the obtained copper indigo pigment, it is always necessary to improve the gloss and coloring strength of the coated article. In the liquid crystal display, the liquid crystal layer sandwiched between the two polarizing plates controls the first one. The polarizing angle of the polarizing plate controls the amount of light transmitted through the second polarizing plate, thereby performing display. The main liquid crystal display device is a display using twisted nematic (TN) type liquid crystal. By providing color filter between the two polarizing plates The LCD enables the LCD display to display colors. In recent years, liquid helium has been shown to be used in televisions and monitors for personal computers. For this reason, there is a growing need for filters with high brightness and high contrast.

濾色器係由在透明基質比如玻璃基質表面上平行或彼 此交叉排列的至少兩種不同色彩的細條狀濾色器片、或者 以恆定順序水平和垂直排列的細濾、色器片組成。該滤色器 片是微細的,即,從數微米到數百微米,而且該濾色哭片 按照每個色彩以預定的陣列系統地排列。 W ’以真空蒸發和喷濺使The color filter is composed of at least two thin strips of color filters of different colors arranged in parallel or on the surface of a transparent substrate such as a glass substrate, or fine filter and color patches arranged horizontally and vertically in a constant order. The color filter sheets are fine, i.e., from a few micrometers to hundreds of micrometers, and the filter color chips are systematically arranged in a predetermined array for each color. W ’ vacuum evaporation and splashing

然而’通常’有顏料分散其中的濾色器通常有光散射的 通常,在彩色液晶顯示器裝置中,以真 用於驅動液晶的透明電極形成在濾色器上 預定方向定向液晶的定向臈形成其上。為 電極和定向膜的性能,通當雲I a 312XP/發明說明書(補件)/95-08/95114255 7 200706604 問題’這是因為顏料擾亂了由液晶控制的偏光角。也就是 說,當光應當被攔截(〇FF狀態)時光洩漏,而當光應當被 •傳輸(0N狀態)時傳輸光被消弱。此時存在的問題是,在 ㈣—狀態之間的顯示器的亮度比(對低 為了實現具有高對比度㈣色器,對包含在濾色器片中 的顏料進行細碎處理。作為細碎顏料的方法,近年來廣泛 地使用上述的溶劑鹽研磨法。 *劑鹽研磨法是在無機鹽比如氯化鈉或硫酸納和具有 高黏度的水溶性有機溶劑比如乙二醇、二伸乙甘醇或聚乙 二醇存在的情況下,經由用揑合機等機械研磨粒子來細碎 粗顏料粒子的方法。溶劑鹽研磨法對細碎和均句化顏料粒 子是有效的。然而,為了實現對渡色器對比度的改進,需 要使用具有比傳統鹽研磨法獲得的顏料粒子更細並且更 均勻的粒子的顏料。 【發明内容】 、本發明的目的是提供—種製備顏料組成物的方法,該方 =克服了傳統分批揑合機出現的問題,如生產規模的限 t次間的質量變化、由於它的開放式結構而混入雜 貝、以及由於產生粉塵而污染工作環境。 本發明的另—個目的是提供—種與習知分批揑合機相However, in general, a color filter in which a pigment is dispersed generally has light scattering. In a color liquid crystal display device, a transparent electrode which is used to drive a liquid crystal is formed to form an orientation of a liquid crystal in a predetermined direction on a color filter. on. For the performance of the electrode and the oriented film, Tonga Yun I a 312XP / Invention Manual (supplement) / 95-08/95114255 7 200706604 Problem 'This is because the pigment disturbs the polarization angle controlled by the liquid crystal. That is, light leaks when light should be intercepted (〇FF state), and transmitted light when light should be transmitted (0N state). The problem at this time is that the brightness ratio of the display between the (four)-states is low (in order to achieve a high contrast (four) color filter, the pigment contained in the color filter sheet is finely processed. As a method of finely pulverizing the pigment, The solvent salt grinding method described above has been widely used in recent years. * The salt grinding method is a water-soluble organic solvent such as ethylene glycol, diethylene glycol or polyethylene in an inorganic salt such as sodium chloride or sodium sulfate and having a high viscosity. In the case where a diol is present, a method of finely pulverizing coarse pigment particles by mechanically grinding the particles with a kneader or the like. The solvent salt grinding method is effective for finely divided and homogenous pigment particles. However, in order to achieve improvement in contrast of the color former It is necessary to use a pigment having finer and more uniform particles than the pigment particles obtained by the conventional salt milling method. SUMMARY OF THE INVENTION An object of the present invention is to provide a method for preparing a pigment composition, which overcomes the conventional Problems with the batch kneading machine, such as the quality change of the production scale within the limit of t times, the mixing of the shellfish due to its open structure, and the generation of powder Dust and pollute the working environment. Another object of the present invention is to provide a kind of mixing machine with a conventional batch kneader

:=更士里的旎1製備具有更細粒子的顏料組成物的方 法’ Μ顏料分散在印刷油黑P .、 1 由墨比如凹印油墨或膠印油墨或者 塗料的載色劑中時,該多 & 涵枓此夠使塗覆品具有高光澤度和 、者強度’而a即使在要求更細的顏料粒子的應用 312XP/發明說明書(補件)/95·08/95114255 8 200706604 用於噴墨印刷或濾色器的油墨時,也可以賦予其 優異的性質。 〃 供^ ^月的另—特殊目的是提供—種在短時間内有效製 “田顏料的方&,該顏料不能經由習知分批揑合機獲 得0 本,明的另一目的是提供一種用於濾色器的著色組成 物、,亥組成物包含具有微細和均勻的粒子的顏料並且能夠 形成具有高對比度的濾色器。 本毛明的另一目的是提供一種經由使用上述著色組成 物而具有高對比度的濾色器。 根據本發明卜其提供一種製備顏料組成物的方法,該 方法匕括用連續揑合機揑合包含有機顏料、水溶性無機 鹽、水溶性有機液體和樹脂的混合物,上述連續揑合機包 括傳動軸、環形固定盤、與固定盤同心而且整個繞傳動軸 的轴旋轉的旋轉盤,以及在固定盤和旋轉盤之間的間隙中 形成的粉碎空間。 根據本發明2,其提供一種製備顏料組成物的方法,該 方法包括用連續揑合機揑合包含有機染料衍生物、蒽醌衍 生物或二畊衍生物、有機顏料、水溶性無機鹽和水溶性有 機液體的混合物,上述每個衍生物都含有選自酞醯亞胺基 曱基、胺基、石黃酸基或叛酸基的至少一個取代基,上述連 績揑合機包括傳動軸、環形固定盤、與固定盤同心而且整 個繞傳動軸的轴旋轉的旋轉盤,以及在固定盤和旋轉盤之 間的間隙中形成的粉碎空間。 312XP/發明說明書(補件)/95-08/95114255 9 200706604 根據本發明3 ’其提供一種用於濾色器的著色組成物, 二包括由透明樹脂、它的先質或它們的混合物組成的顏料 載體和顏料,其中該顏料包含經由用連續捏合機捏合包含 L有機顏料、水洛性無機鹽和水溶性有機液體的混合物而獲 =的彳政細有機顏料,上述連續揑合機包括傳動軸、環形固 疋盤、與固定盤同心而且整個繞傳動轴的轴旋轉的旋轉 盤,以及在固定盤和旋轉盤之間的間隙中形成的粉碎空 間。 春本發明還提供-種包括由上述著色組成物形成的遽色 器片的濾色器。 (發明效果) 根據由本發明提供的製備顏料組成物的方法,與習知分 批揑合機相比生產規模的限制較小,因此適量的及時生產 疋可能的。此外,本發明的方法還具有以下優點。產品批 次之間的質量變化較小。由於使用的揑合機是密閉式揑合 _機,因此可以克服由於產生粉塵而污染工作環境和混入雜 質的問題。粒子可以以少量的能量粉碎成微細粒子。當由 本發明的方法獲得的有機顏料分散在油墨如凹印油墨或 膠印油墨或者塗料中時,顏料給予塗覆品良好的光澤度和 改進的著色強度。此外,特別適合在要求透明度的應用中。 根據由本發明提供的用於濾色器的著色組成物,由於該 著色組成物包含通常難以獲得的具有均勻粒徑的微細Z 子的有機顏料,因此使用本發明的著色組成物能夠形成對 比度較以往更南的滤色裔。 312XP/發明說明書(補件)/95-08/95114255 10 200706604 【實施方式】 百先’參照圖1說明用在本發明 是顯示用在本發明中的連續揑合機具體;= 圖。作為用在本發明φ沾、*你,^ A w的剖面側視 用JP-B 2 92 Φ 績揑合機的較佳例子,可以使 .,. 中么開的連續揑合機。例如,較佳使用由 l〇(「Miracle K.C.K.」復的連續揑合機 如圖1所^連續揑合機1G具有包 合部分2、出料部分3和計量加料器部分4=二士广 加料部分1包括水平方向延 刀4±的基本結構。 11同心並以滑動接觸狀能壯 /卜喊11和與外殼 ^闕狀㈣配的螺 加料器部分4接收原料的原料入口⑴門口/於攸e十里 殼11的頂面。螺旋桿12的起動端汗上游側的外 固定到驅動電動機的傳動轴121(圖^省7)被同心, 助驅動電動機的驅動經由傳動軸121 ,而且猎 ❿ 12繞傳動軸121的軸旋轉 々媒:1 ’使得螺旋桿 旋形翅片122安裝在螺旋桿二向形成螺旋形的螺 翅片122的繞軸旋轉,由計斗::上。藉助螺旋形 強有力地提供至揑合部分2。 / °σ5?4供給的原料被 安裝計量加料器部分4, 的原料(在本發明中為包含有嬙e、,P將進仃連續揑合處理 溶性有機液體和樹脂或有機料顏1、水溶性無機鹽、水 口井衍生物的溶膠或凝膠現合物4何生物、蒽酿衍生物或三 組成物」)提供至加料部分】在下文中有時稱作「揑合 甲。計量加料器部分4包括 312XP/發明說明書(補件)/9M)8/95114255 200706604 ==斗41、將來自於原料漏斗41底部的原 二中的螺旋加料器42、和自外殼η中 出口端的連接圓柱體43。 疋加科益42 44安/動ΓΓTV2以使它的螺旋形翅片與中間圓柱體 開口和連接圓柱體43的上部 寸41的底# 起動端(圖1的右側)同心連二:螺:加料器42的 的值叙击“ 連接在圖1中痛略的進給電動機 的傳動軸上。因此,藉助於由於進 电助械 的螺旋加料器42的繞轴旋轉,用螺 '的:動而引起 斗41中的原料以預定的傳送量通過中間圓:體η: 圓柱體43傳送到外殼η中。 W柱體44和連接 揑合部分2包括多個固定盤21、 的環形揑合圓筒22、和旋轉盤23 定盤w21之間 圓筒22交錯設置,旋轉盤2 21和壞形揑合 的古hw 、 則表面和後表面(圖1中 =表面和左表面)與固定盤21相 二 圓向?。圖!中省略的拉桿插入穿過上述;:二 21和捏合圓筒22。拉桿的固 口疋盤 殼11上。因而,固定般Μ疋在加料部分1的外 結合。 固疋盤21和捏合圓筒22與加料部分i 各個旋轉盤23裝配在栓槽轴(圖 旋桿12❼最前部表面同心伸出 ^略)中’其從螺 在每兩個相鄰的旋轉盤23之間。^ ^螺# 24安褒 24交錯安裝在栓槽軸上。旋 外=轉盤23和螺桿 疋褥4 23的外徑稍小於揑合圓 312^mmmmm/95^08/95114255 12 200706604 筒22的内徑’中間螺桿24的外徑稍小於固定盤21的内 徑。由於這個原因,在旋轉盤23和中間螺桿24交錯裝配 於栓槽軸上的情況下,各個旋轉盤23和各個申間螺桿"24 的外圓周表面通過原料能夠通過的間隙分別與揑合圓筒 22和固定盤21的内圓周表面相對。 由於連縯揑合機ίο的上述構造,藉助於螺旋加料器42 的驅動,位於原料漏斗41甲的原料被從原料漏斗41的底 部取出,然後通過中間圓柱體44和連接圓柱體43引入到 加料部分1的外殼n中。藉助於由於螺旋桿12的驅動旋 轉而引起的螺旋形翅片122的旋轉,引入到外殼u中的 原料在下游側被連續地傳送到揑合部分2中。 然後,使傳送到揑合部分2中的原料首先通過最上游側 ⑽1中的右側)繞軸旋轉的中間螺桿24的外圓周表面和 攻上游侧的固定盤21 _圓周表面之間的間隙 原料通過圖!中最上游側的固定盤21的左側表面:最上 游側繞軸旋轉的旋轉盤23的右侧表面之間的間隙。當原 ^通過這些間隙時’該原料被揑合。根據固^ 二圓=2、旋轉盤23和中間螺桿24安裝的數量在多^ 白=稷對原料的上述操作。由於這個原因,原料的多種 發明中的有機顏料、水溶性無機鹽和水溶性有機 =受°=機Γ!衍生物,衍生物或三*生物) 出料邻八3 疋成揑合處理獲得的產品從間隙、即 外圓周表面和位於最下游側的旋轉盤23的 取下游側的揑合圓筒22的内圓周表面 312XP/發明說明書(補件)/95_〇8/95114255 13 200706604 之間。 圖2顯示了用於圖丨所示連續揑合具體例的固定盤和旋 轉盤的前視圖(從圖1的右側觀察)或後視圖(從圖丨的左 側觀察)。在圖2中,(a)是空腔扇形固定盤21a,(b)是 空腔扇形旋轉盤23b,(c)是空腔玫瑰形固定盤2ic,(d) 疋空腔玫瑰形旋轉盤23d,(e)是空腔臼形固定盤21 e,(f) 是空腔臼形旋轉盤23f。 如圖2所示,每個固定盤21具有與中間螺桿24同心的 活動裝配孔211,其中中間螺桿24將被鬆動地裝配。在 /舌動t配孔211的徑向,多個凹口(空腔(粉碎空間)212 ) 在每個固定盤21的前表面和後表面(前視側和後視侧)上 形成中空,在周向以規則間距提供這些凹口。在另一方 面,各個旋轉盤23具有與栓槽軸同心的裝配孔231,其 中以遂切接觸的方式裝配圖1中省略的栓槽軸。與固定盤 21的空腔212相對應的空腔(粉碎空間)232在各個旋轉盤 23的前表面和後表面上形成中空。旋轉盤23的各個空腔 2 3 2的邊緣是打開的。 由於螺旋桿12的驅動,將引入到固定盤21和旋轉盤 23之間的間隙的原料連續推進到相應的空腔212和232 中。在該狀態下,在空腔212和232的介面上,繞軸旋轉 的方疋轉盤23在空腔212和232中的原材料上產生了剪切 力。也就是說’用空腔212和232的山脊部分切開彼此相 對的固定盤21的空腔212和旋轉盤2 3的空腔2 3 2中的原 料’從而在原料上產生剪切力並且進行置換,由此揑合和 312XP/發明說明書(補件)/95-〇g/95114255 14 200706604 分散該原料。在上述置換過程中,被剪切原料離開空腔 212和232而新原料進入同一空腔212和232。 根據空腔212和232的形狀,固定盤21和旋轉盤23分 為多個不同種類的固定盤和旋轉盤。也就是說,它們分別 進入圖2中的(a)和(b)所示的空腔扇形固定盤21a和空腔 扇形旋轉盤23b、圖2中(b)和(c)所示的空腔玫瑰形固定 盤21c和空腔玫瑰形旋轉盤23d、以及圖2中的(幻和(〇 所不的空腔臼形固定盤21 e和空腔臼形旋轉盤23f。這些 不同種類的固定盤和旋轉盤用於根據揑合和分散處理= 進度增加作用於原料的剪切力。 也就是說,從最高到最低,空腔212或232的空隙率等 級順序(固定盤21的空腔212或旋轉盤23的空腔232的 面積基於固定盤21或旋轉盤23的表面積的百分率(%)) 是扇形空腔212或232、玫瑰形空腔212或232、和臼形 空腔212和232。作用於原料的剪切力隨空隙率的降低 增加。 - 在該具體例中,從上游側到下游侧順序配置具有扇形空 腔212的固定盤21和具有扇形空腔232的旋轉盤23·且 有玫瑰形空腔212的固定盤21和具有玫瑰形空二2犯= 旋轉盤23;以及具有臼形空腔212的固定盤以和具有臼 形空腔232的旋轉盤23,以使作用於原料的剪切力' 揑合和分散處理原料的進度增加。 如此,大的t切力不會突然施加於原料,而是隨著 的揑合和分散處理的進行,連續地增加作用於原料的剪切 312XP/發明說明書(補件)/95-08/95114255 Η 200706604 力。因此,在沒有任何額外應變的情況下,將揑合和分散 處理平穩地施加於原料。因而,能夠使均為原料組分的有 機顏料、水溶性無機鹽、水溶性有機液體和樹脂或有機染 料衍生物、恩醌衍生物或三讲衍生物成功地相互揑合和分 散。 根據具有這種結構的連續揑合機1 〇,當作為原料組分 的有機顏料由粗粒子組成時,通過將有機顏料引入到固定 盤21和旋轉盤23之間的間隙(尤其是,空腔212和232) 中並藉助於旋轉盤23的旋轉向該粗粒子施加剪切力,能 夠將有機顏料的粗粒子粉碎成微細粒子。 另一方面,當有機顏料由微細粒子的聚集體組成時,經 由將這些聚集體引入到固定盤21和旋轉盤23之間的間隙 (尤其是,空腔212和232)中並旋轉旋轉盤23,能夠穩定 地裂化和均勻這些聚集體。 將在下文詳細說明用上述連續揑合機丨〇揑合和分散的 顏料。通過用連續揑合機10揑合包含有機顏料、水溶性 無機鹽、水溶性有機液體和樹脂的混合物來獲得本發明i 的顏料組成物,連續揑合機10包括傳動軸121、環形固 定盤21、與固定盤21同心並整個繞傳動軸121的軸旋轉 的旋轉盤23,和在固定盤21和旋轉盤23之間的間隙中 形成的粉碎空間。 用在本發明中的有機顏料是指在合成時選擇適當的反 應條件而使其粒子尺寸微細和均勻的有機顏料,如偶氮顏 料;在後處理中、其合成中產生的成塊極細粒子生長後^ 312χρ/發明說明書(補件)/95-08/95114255 16 200706604 使其粒子尺寸均句的有機顏料,如多i化的麻青顏料; 以及在後處理中,通過細碎粒子能夠使在它的合成中產生 的粗粒和不均勻粒子的尺寸均勻的有機顏料,如銅酿青顏 料此外,5亥有機顏料在結構上不受特別限制,只要它是 在尺寸上需要細碎和均句的顏料即可。該有機顏料可以選 自習知的有機顏料。有機顏料的例子包括偶氮顏料、敝青 顏料和啥°丫_顏料,而且還包括異,嗓啉綱、異t朵啉、 二萘嵌苯、茈酮、二酮吡咯並吡咯、硫靛藍、二哼畊、喹 諾酞酮、蒽靦和觳蒽酿。可微細地粉碎至少兩種有機顏料 的混合物。 用在本發财的水溶性無機鹽不受特職f卜它的例子 包括食鹽(氯化納)、氯化鉀、硫酸鈉、氯化鋅、氯化飼以 及匕們的混合物。 甲基醚、二伸乙甘醇一乙基醚 添加用在本發明中的水溶性有機液體,以使有機顏料和 水溶性無機鹽形成均句的漿體。水溶性有機液體不受特別 限制,只要它可與水自由混合、或者即使它不能與水自由 :δ仁/、有月b夠通過I業水洗而被去除的溶解度、並且 還允許顏料粒子生長即可。由於揑合期間溫度升高,該液 體傾向於易於蒸發。為此,考慮到安全性較佳係高沸點 劑。例如包括2-(甲氧基)乙醇、2_ 丁氧基乙醇、2_( 氧基)乙醇、2-(己氧基)乙醇、二伸乙甘醇、二伸乙甘醇 乙甘醇一丁基_、 三伸乙甘醇、三伸乙甘醇一甲基醚、液態聚乙二醇、工 甲氧基-2-丙醇、卜乙氧基_2_丙醇、二丙二醇、二丙二醇 312XP/發明說明書(補件)/95-08/95114255 17 200706604 曱基醚、一丙二醇一乙基醚、低分子量的聚丙 胺、吼咬、四氫吱喃、二氧六環、甲醇、乙醇、異丙醇、 正丙醇、異丁醇、正丁醇、乙二醇、丙二醇、丙二醇一甲 基醚醋酸醋、乙酸乙賴、乙酸異丙醋、丙酮、甲乙酮、二 曱基甲S&胺、二曱亞颯和N_甲基吡咯烷酮。根據需要可 以使用至少兩種有機液體的混合物。 用在本叙明中的树脂較佳是難溶於水、在室溫下是液體 1口體而且部分溶於本發明所用的水溶性有機液體的樹 月曰。例如包括松香樹脂如松香、歧化松香、聚合松香、氫 化权曰争A香酉曰、松香胺、馬來酸改性松香、富馬酸改性 松香、松香金屬鹽、松香改性祕樹脂和松香改性馬來酸 樹脂,合成樹脂如環氧樹脂、丙稀酸樹脂、馬來酸樹脂、 :酸樹脂、聚醋樹脂、三聚氰胺樹脂、酴盤樹脂、聚胺醋 树脂和聚醯胺樹脂,以及衍生自纖維素、橡膠等的改性樹 脂。尤其是,考慮到添加的效果和價格,較佳松香樹脂。 本發明揑合組成物中的水溶性無機鹽的量不受特別限 #曰1。水溶性無機㈣量較佳為有機顏料量$ 〇 5到加 量倍。當其小於0.5重量倍時,細碎是困難的。當1大於 ^重量倍時,有可能獲得細碎顏料,但處理的顏料量變 侍較小,以致於在工業方面不利地降低了生產率。 312XP/發明說明書(補件),95·〇8/95114255 本發明揑合組成物㈣水溶性有機液體的量不 限制^溶性有機液體的量較佳為有機顏料和水溶性= 鹽總篁的0.01到0.5重量倍。當其小於〇 〇i重量倍時, 揑合組成物變得過硬以致於難以穩定操作。當其大重 200706604 虽L日守,揑合組成物變得過軟以致於細碎的程度降低。 此外,本發明揑合組成物中的樹脂的量不受特別限制。 树月曰的1較佳為有機顏料重量的〇· 〇〇丨到1 · 〇倍。當其重 量小於〇· 001倍時,不能達到添加的效果。當其重量大於 1 · 0 L日守’不此達到與樹脂的添加量相應的效果。此外, 2佳根據所得顏料組成物使用的樹脂和載色劑樹脂的性 質,異控制樹脂的量。也就是說,當差異較大時,以最小 的量使用該樹脂,以減少對載色劑樹脂物理性質的影響。 另方面,當差異較小時,較佳增加該樹脂的量以充分顯 示本發明的效果。 1 作為本發明1揑合組成物的組分的有機顏料、水溶性益 ,鹽、水溶性有機液體和樹脂可以同時分別添加到連續揑 -機中另外這些組分可以在混合後添加到連續揑合機 中此外,還有可能在製備有機顏料的過程中添加樹脂以 便預先开7成有機顏料和樹脂的混合物。在該情況下,顯著 地主現出樹脂的添加效果。 本發明2涉及-種製備顏料組成物的方&,該方法包括 用連續揑合機揑合包含有機㈣衍生物、1靦衍生物或三 °井何生物、有機顏料、水溶性無機鹽和水溶性有機液體的 混合^,上述各個衍生物都含有選自酞醯亞胺基甲基、胺 基、績酸基或㈣基的至少—個取代基,上述連續捏合機 包括傳動軸、環形固定盤、與岐盤同心而且整個繞傳動 軸的軸旋轉的旋轉盤’以及在固定盤和旋轉盤之間的間隙 中形成的粉碎空間。 312XP/發明說明書(補件 y95_〇8/95114255 19 200706604 用在本發明2中的含有至少一個選自酞醯亞胺基甲 基、胺基、磺酸基或羧酸基的取代基的有機染料衍生物典 -型地是由下述式(1)代表的有機染料衍生物, - P-{Xi-(Yi)k}m ⑴ 其中P表示有機染料殘基;Χι是單鍵或表示_〇_、-S-、 -⑶-、-S〇2-、-、-C0NR广、-SOAR^、-NRlC〇-或 NRJOr、 具有1到12個碳原子的線性或支鏈亞烴基'可以被烷基、 胺基、硝基、羥基、烷氧基或_原子取代的苯或三讲殘基, 或者由至少兩個這些連接基團組成的聯合連接基團,其中 h表示氫原子、烷基或羥烷基;1是可以被硝基或鹵原子 取代的酞醯亞胺基曱基、一NR2r3、—s〇3 · M/n或一c〇〇 · M/n ; 其中R2和R3每一個單獨表示氫原子、取代或未取代的烷 基、取代或未取代的稀基或取代或未取代的苯基,或者 R2和R3 —起形成取代或未取代的雜環,該雜環可以包含另 外的氮原子、氧原子或硫原子,Μ表示氫離子、化合價為 _ 1到3的金屬離子或被至少一個烷基取代的銨離子,η是 Μ的化合價,k是1或2的整數;m是從1到4的整數。 用在本發明2中的含有至少一個選自酞醯亞胺基曱基、 胺基、石頁酸基或叛酸基的取代基的蒽酿衍生物典型地是由 下述式(2)表代表的恩醒衍生物, Q-{X2-(Y2)k}m (2) 其中Q表示可以被烷基、胺基、硝基、羥基、烷氧基或 鹵原子取代的恩酿殘基;X2是單鍵或表示—Ο—、、—Co—、 -SO2-、-NRi-、-CONRi-、-S〇2NR丨-、-NRiCO-或 NRiS〇2-,具 312XP/發明說明書(補件)/95-08/95114255 20 200706604 ^ 1到12個碳原子的線性或支鏈亞烴基,可以被烧基、 胺基、靖基、㉙基、絲基或㈣子取代的苯或三韻基, 或者由至少兩個這些連接基團組成的聯合連接基團,其中: = Method for preparing a pigment composition having finer particles in the 旎 1 of the damster' Μ The pigment is dispersed in the printing oil black P., 1 when the ink is in a vehicle such as a gravure ink or an offset ink or a coating, Multi & 枓 够 够 够 够 够 够 够 够 够 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 涂覆 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 312 Inkjet printing or color filter inks can also impart excellent properties.另 Another special purpose for ^ ^ month is to provide a kind of "field paint" in a short time, the pigment can not obtain 0 through the conventional batch kneader, another purpose of Ming is to provide a A coloring composition for a color filter, a composition comprising a pigment having fine and uniform particles and capable of forming a color filter having high contrast. Another object of the present invention is to provide a coloring composition by using the above-described coloring composition A color filter having high contrast. According to the present invention, there is provided a method for preparing a pigment composition, which comprises kneading a mixture comprising an organic pigment, a water-soluble inorganic salt, a water-soluble organic liquid and a resin by a continuous kneader. The above continuous kneader includes a drive shaft, an annular fixed disk, a rotary disk that is concentric with the fixed disk and rotates entirely around the axis of the drive shaft, and a pulverizing space formed in a gap between the fixed disk and the rotary disk. According to the present invention 2, It provides a method of preparing a pigment composition, which comprises kneading an organic dye derivative, an anthracene derivative, by a continuous kneader a mixture of a second ploughing derivative, an organic pigment, a water-soluble inorganic salt, and a water-soluble organic liquid, each of which contains at least one selected from the group consisting of a fluorenylene sulfhydryl group, an amine group, a rhein acid group, or a tick acid group. In one alternative, the above-described continuous kneading machine includes a drive shaft, an annular fixed disk, a rotary disk that is concentric with the fixed disk and rotates entirely around the axis of the drive shaft, and a pulverizing space formed in a gap between the fixed disk and the rotary disk. 312XP / Invention specification (supplement) / 95-08/95114255 9 200706604 According to the invention 3' it provides a colored composition for a color filter, two comprising a transparent resin, its precursor or a mixture thereof a pigment carrier and a pigment, wherein the pigment comprises a quinone fine organic pigment obtained by kneading a mixture comprising an L organic pigment, a watery inorganic salt and a water-soluble organic liquid by a continuous kneader, the continuous kneader comprising a drive shaft, An annular solid disc, a rotating disc concentric with the fixed disc and rotating around the shaft of the drive shaft, and a crushing space formed in a gap between the fixed disc and the rotating disc The present invention also provides a color filter including a color filter sheet formed of the above colored composition. (Effect of the Invention) According to the method for producing a pigment composition provided by the present invention, compared with a conventional batch kneader The production scale is less restrictive, so an appropriate amount of timely production is possible. In addition, the method of the present invention has the following advantages: the mass variation between product batches is small. Since the kneading machine used is a closed kneading machine, Therefore, it is possible to overcome the problem of contaminating the working environment and mixing impurities due to the generation of dust. The particles can be pulverized into fine particles with a small amount of energy. When the organic pigment obtained by the method of the present invention is dispersed in an ink such as a gravure ink or an offset ink or paint The pigment imparts good gloss and improved color strength to the coated article. Further, it is particularly suitable for applications requiring transparency. According to the colored composition for a color filter provided by the present invention, it is generally difficult to contain the colored composition. Obtaining an organic pigment having a fine particle size of a uniform Z, thus using the coloring composition of the present invention It is capable of forming a filter color that is more south than the past. 312XP/Invention Manual (Supplement)/95-08/95114255 10 200706604 [Embodiment] The first embodiment is described with reference to Fig. 1 for use in the present invention to show a continuous kneader for use in the present invention; As a preferred example of the JP-B 2 92 Φ kneading machine used for the cross-sectional side of the present invention, it is possible to use a continuous kneading machine which is opened in . For example, it is preferred to use a continuous kneader consisting of "Miracle KCK" as shown in Fig. 1. The continuous kneading machine 1G has a clad portion 2, a discharge portion 3, and a metering feeder portion 4 = a widened portion 1 It includes the basic structure of the horizontal knives 4±. 11 Concentric and slidable contact can be strong and shouted 11 and the screw feeder part 4 with the outer casing (4) receives the raw material inlet (1) doorway / Yu 攸e Shili The top surface of the casing 11. The drive shaft 121 (Fig. 7) externally fixed to the driving motor on the upstream side of the starting end of the auger 12 is concentric, the driving of the driving motor is transmitted via the transmission shaft 121, and the hunting wheel 12 is wound. The shaft of the shaft 121 rotates the medium: 1 ' so that the spiral-arc fins 122 are mounted on the pivot of the spiral-shaped spiral fins 122 in the two directions of the spiral shaft, and are supported by the bucket: Provided to the kneading portion 2. The raw material supplied from the / ° σ 5 ? 4 is supplied with the raw material of the metering feeder portion 4 (in the present invention, 嫱e is contained, P is continuously kneaded to process the soluble organic liquid and the resin or organic Material 1, water-soluble inorganic salt, water well derived The sol or gel present compound 4), which is supplied to the feed portion, is sometimes referred to as "kneading". The metering feeder portion 4 includes the 312XP/invention specification (supplement) /9M)8/95114255 200706604 == bucket 41, the screw feeder 42 from the bottom of the raw material funnel 41, and the connecting cylinder 43 from the outlet end of the outer casing η. 疋加科益42 44A/ The TV2 is moved such that its spiral fin is concentric with the intermediate cylinder opening and the bottom end of the upper inch 41 of the connecting cylinder 43 (the right side of FIG. 1): the value of the screw: the loader 42 is " Connected to the drive shaft of the feed motor shown in Figure 1. Therefore, by means of the pivoting of the screw feeder 42 due to the power feeding, the material in the bucket 41 is caused to pass through the intermediate circle with a predetermined amount of conveyance by the movement of the screw: the body η: the cylinder 43 is conveyed to the outer casing η. The W cylinder 44 and the connection kneading portion 2 include a plurality of fixed discs 21, a ring-shaped kneading cylinder 22, and a rotating disc 23, and the cylinders 22 are alternately disposed between the cylinders 22, the rotating discs 21 and the badly kneaded ancient hw, Then the surface and the back surface (in Fig. 1 = surface and left surface) are in a circular direction with the fixed disk 21? . Figure! The rod that is omitted in the middle is inserted through the above; two 21 and the kneading cylinder 22. The solid rod of the tie rod is mounted on the casing 11. Thus, the outer joint of the feeding portion 1 is fixed. The fixing disk 21 and the kneading cylinder 22 and the feeding portion i are respectively mounted on the swash plate shaft (the front end surface of the rotating rod 12 同 is concentrically extended), and the snail is screwed on every two adjacent rotating disks. Between 23 . ^ ^螺# 24 Ampoules 24 staggered mounted on the pinch shaft. The outer diameter of the outer turn = turntable 23 and the screw 疋褥 4 23 is slightly smaller than the kneading circle 312^mmmmm/95^08/95114255 12 200706604 The inner diameter of the cylinder 22 The outer diameter of the intermediate screw 24 is slightly smaller than the inner diameter of the fixed disk 21. For this reason, in the case where the rotary disk 23 and the intermediate screw 24 are alternately mounted on the pin groove shaft, the outer circumferential surfaces of the respective rotary disks 23 and the respective inter-spindle screws "24" respectively pass through the gap through which the raw material can pass and the kneading cylinder 22 is opposed to the inner circumferential surface of the fixed disk 21. Due to the above configuration of the kneading machine ίο, the raw material of the raw material funnel 41A is taken out from the bottom of the raw material funnel 41 by the driving of the screw feeder 42, and then introduced into the feeding portion through the intermediate cylinder 44 and the connecting cylinder 43. 1 in the outer casing n. The raw material introduced into the outer casing u is continuously conveyed to the kneading portion 2 on the downstream side by the rotation of the spiral fin 122 due to the driving rotation of the auger 12. Then, the raw material conveyed to the kneading portion 2 is first passed through the outer circumferential surface of the intermediate screw 24 which is rotated about the right side in the most upstream side (10) 1 and the gap between the outer circumferential surface of the upstream disk and the fixed disk 21_circumferential surface ! The left side surface of the fixed disk 21 on the most upstream side is the gap between the right side surfaces of the rotary disk 23 which is rotated about the axis on the most upstream side. When the original passes through these gaps, the material is kneaded. According to the number of solid two rounds = 2, the rotating disk 23 and the intermediate screw 24 are installed in the above-mentioned operation of the raw material. For this reason, organic pigments, water-soluble inorganic salts, and water-soluble organic substances in various inventions of raw materials are obtained by kneading the adjacent eight-dimensional kneading process. From the gap, that is, the outer circumferential surface and the inner circumferential surface 312XP of the kneading cylinder 22 on the downstream side of the rotary disk 23 on the most downstream side, between the invention specification (supplement)/95_〇8/95114255 13 200706604. Fig. 2 shows a front view (viewed from the right side of Fig. 1) or a rear view (viewed from the left side of the figure) of the fixed disk and the rotary table for the continuous kneading of the specific example shown in Fig. 2. In Fig. 2, (a) is a cavity sector-shaped fixed disk 21a, (b) is a cavity sector-shaped rotating disk 23b, (c) is a cavity rose-shaped fixed disk 2ic, (d) a cavity-shaped rose-shaped rotating disk 23d (e) is a cavity-shaped fixed disk 21 e, and (f) is a cavity-shaped rotating disk 23f. As shown in Fig. 2, each of the fixed disks 21 has a movable fitting hole 211 concentric with the intermediate screw 24, in which the intermediate screw 24 is to be loosely fitted. In the radial direction of the / tongue t-aligning hole 211, a plurality of recesses (cavities (shrinking spaces) 212) are formed in a hollow shape on the front and rear surfaces (front side and rear side) of each of the fixed disks 21, These notches are provided at regular intervals in the circumferential direction. On the other hand, each of the rotary disks 23 has a fitting hole 231 concentric with the bolt groove shaft, in which the bolt groove shaft omitted in Fig. 1 is assembled in a chopped contact manner. A cavity (shredding space) 232 corresponding to the cavity 212 of the fixed disk 21 is formed hollow on the front and rear surfaces of the respective rotary disks 23. The edges of the respective cavities 2 3 2 of the rotary disk 23 are open. Due to the driving of the auger 12, the material introduced into the gap between the fixed disk 21 and the rotary disk 23 is continuously advanced into the respective cavities 212 and 232. In this state, at the interface of the cavities 212 and 232, the pivoting turntable 23 produces shearing forces on the raw materials in the cavities 212 and 232. That is to say, 'the ridge portion of the cavities 212 and 232 partially cuts the cavity 212 of the fixed disk 21 opposed to each other and the material 2' in the cavity 2 3 of the rotating disk 2 3 to thereby generate shear force and replace the material on the raw material. Thus, the kneading and 312XP/invention specification (supplement)/95-〇g/95114255 14 200706604 disperse the raw material. During the above replacement process, the sheared material exits the cavities 212 and 232 and the new material enters the same cavity 212 and 232. Depending on the shape of the cavities 212 and 232, the fixed disk 21 and the rotary disk 23 are divided into a plurality of different kinds of fixed disks and rotating disks. That is, they respectively enter the cavity sector-shaped fixed disk 21a and the cavity sector-shaped rotating disk 23b shown in (a) and (b) of Fig. 2, and the cavities shown in (b) and (c) of Fig. 2, respectively. a rose-shaped fixed disk 21c and a cavity rose-shaped rotating disk 23d, and in FIG. 2 (the phantom and the cavity-shaped fixed disk 21 e and the cavity-shaped rotating disk 23f. These different kinds of fixed disks And the rotating disk is used to increase the shearing force acting on the raw material according to the kneading and dispersion treatment = progress. That is, from the highest to the lowest, the void ratio of the cavity 212 or 232 is sequentially ordered (the cavity 212 of the fixed disk 21 or the rotation) The area of the cavity 232 of the disk 23 is based on the percentage (%) of the surface area of the fixed disk 21 or the rotary disk 23) is a sector-shaped cavity 212 or 232, a rose-shaped cavity 212 or 232, and a dome-shaped cavity 212 and 232. The shearing force of the raw material increases as the void ratio decreases. - In this specific example, the fixed disk 21 having the sector-shaped cavity 212 and the rotating disk 23 having the sector-shaped cavity 232 are sequentially disposed from the upstream side to the downstream side and have a fixed disk 21 of the rose-shaped cavity 212 and having a rose-shaped void 2 2 = rotating disk 23; The fixed disk of the shaped cavity 212 and the rotating disk 23 having the dome-shaped cavity 232 increase the progress of the shearing force acting on the raw material to knead and disperse the raw material. Thus, the large t shear force is not suddenly applied. In the raw material, but with the progress of the kneading and dispersion treatment, the shearing action on the raw material is continuously increased 312XP / invention specification (supplement) / 95-08/95114255 Η 200706604 force. Therefore, without any additional strain In this case, the kneading and dispersion treatment are smoothly applied to the raw material. Thus, the organic pigment, the water-soluble inorganic salt, the water-soluble organic liquid and the resin or the organic dye derivative, the enema derivative or the three which are all raw material components can be obtained. The derivative is successfully kneaded and dispersed with each other. According to the continuous kneader 1 having such a structure, when the organic pigment as a raw material component is composed of coarse particles, by introducing the organic pigment to the fixed disk 21 and the rotary disk 23 The gap between the gaps (especially, the cavities 212 and 232) is applied to the coarse particles by the rotation of the rotary disk 23, and the coarse particles of the organic pigment can be pulverized into fine particles. On the other hand, when the organic pigment is composed of aggregates of fine particles, by introducing these aggregates into the gap between the fixed disk 21 and the rotary disk 23 (particularly, the cavities 212 and 232) and rotating the rotary disk 23 It is possible to stably crack and homogenize these aggregates. The pigment kneaded and dispersed by the above-described continuous kneader will be described in detail below by kneading an organic pigment, a water-soluble inorganic salt, a water-soluble organic liquid, and the like by a continuous kneader 10 A mixture of resins for obtaining the pigment composition of the present invention i, the continuous kneading machine 10 comprising a drive shaft 121, an annular fixed disk 21, a rotary disk 23 concentric with the fixed disk 21 and rotating around the axis of the drive shaft 121, and a fixed disk The pulverizing space formed in the gap between 21 and the rotary disk 23. The organic pigment used in the present invention refers to an organic pigment which is selected to have appropriate reaction conditions during synthesis to make the particle size fine and uniform, such as an azo pigment; in the post-treatment, the synthesis of agglomerated extremely fine particles After ^ 312 χ ρ / invention manual (supplement) / 95-08/95114255 16 200706604 organic pigments that make the particle size uniform, such as multi-colored phlegm pigment; and in the post-treatment, through the fine particles can make it in it An organic pigment having a uniform size of coarse particles and uneven particles produced in the synthesis, such as a copper-brown cyanine pigment. In addition, the organic pigment of 5H is not particularly limited in structure, as long as it is a pigment which requires finely divided and uniform in size. Just fine. The organic pigment can be selected from conventional organic pigments. Examples of the organic pigment include an azo pigment, an indigo pigment, and a quinone pigment, and also include an iso, porphyrin, iso-t-porphyrin, perylene, anthrone, diketopyrrolopyrrole, thioindigo, Two tillage, quinolone, anthraquinone and brewing. The mixture of at least two organic pigments can be finely pulverized. The water-soluble inorganic salt used in the present invention is not particularly useful as an example of salt (sodium chloride), potassium chloride, sodium sulfate, zinc chloride, chlorinated feed, and mixtures thereof. Methyl Ether, Diethylene Glycol Monoethyl Ether The water-soluble organic liquid used in the present invention is added so that the organic pigment and the water-soluble inorganic salt form a uniform slurry. The water-soluble organic liquid is not particularly limited as long as it can be freely mixed with water, or even if it cannot be freed with water: δ kernel /, the solubility which is removed by the I industry water washing, and allows the growth of the pigment particles, that is, can. The liquid tends to evaporate easily due to an increase in temperature during kneading. For this reason, it is preferable to use a high boiling point agent in consideration of safety. For example, 2-(methoxy)ethanol, 2-butoxyethanol, 2-(oxy)ethanol, 2-(hexyloxy)ethanol, diethylene glycol, diethylene glycol, ethylene glycol monobutyl _, triethylene glycol, triethylene glycol monomethyl ether, liquid polyethylene glycol, methoxy-2-propanol, ethoxylated 2-propanol, dipropylene glycol, dipropylene glycol 312XP /Invention Manual (Supplement)/95-08/95114255 17 200706604 Mercaptoether, monopropylene glycol monoethyl ether, low molecular weight polypropylamine, bite, tetrahydrofuran, dioxane, methanol, ethanol, iso Propyl alcohol, n-propanol, isobutanol, n-butanol, ethylene glycol, propylene glycol, propylene glycol monomethyl ether acetate vinegar, acetic acid, isopropyl acetate, acetone, methyl ethyl ketone, dimercapto S & amine, Diterpenoids and N-methylpyrrolidone. A mixture of at least two organic liquids can be used as needed. The resin used in the present description is preferably a tree which is hardly soluble in water, is a liquid at room temperature, and is partially soluble in the water-soluble organic liquid used in the present invention. Examples include rosin resins such as rosin, disproportionated rosin, polymerized rosin, hydrogenated hydrazine, rosin, maleic acid modified rosin, fumaric acid modified rosin, rosin metal salt, rosin modified resin and rosin. Modified maleic acid resin, synthetic resin such as epoxy resin, acrylic resin, maleic acid resin, acid resin, polyester resin, melamine resin, enamel resin, polyurethane resin and polyamide resin, and A modified resin derived from cellulose, rubber, or the like. In particular, rosin resins are preferred in view of the added effect and price. The amount of the water-soluble inorganic salt in the kneaded composition of the present invention is not particularly limited to #曰1. The amount of the water-soluble inorganic (tetra) is preferably from 〇 5 to an additional amount of the organic pigment. When it is less than 0.5 weight times, fine crushing is difficult. When 1 is more than ^ times the weight, it is possible to obtain a finely divided pigment, but the amount of the pigment to be treated becomes less so that the productivity is disadvantageously lowered industrially. 312XP/Invention Manual (Supplement), 95·〇8/95114255 The kneaded composition of the present invention (IV) The amount of the water-soluble organic liquid is not limited. The amount of the soluble organic liquid is preferably 0.01% of the organic pigment and water-soluble = total salt of the salt. 0.5 weight times. When it is less than 重量i by weight, the kneaded composition becomes too hard to be stably handled. When it is heavy, 200706604 Although the L is kept, the kneading composition becomes so soft that the degree of fine crushing is reduced. Further, the amount of the resin in the kneaded composition of the present invention is not particularly limited. The sap of the tree sorghum is preferably 1·〇〇丨 to 1 〇 times the weight of the organic pigment. When the weight is less than 001· 001 times, the added effect cannot be achieved. When the weight is greater than 1 · 0 L, the day's do not achieve the effect corresponding to the amount of resin added. Further, it is preferable to control the amount of the resin depending on the properties of the resin used in the obtained pigment composition and the vehicle resin. That is, when the difference is large, the resin is used in a minimum amount to reduce the influence on the physical properties of the vehicle resin. On the other hand, when the difference is small, the amount of the resin is preferably increased to sufficiently exhibit the effects of the present invention. 1 as an ingredient of the kneading composition of the present invention, an organic pigment, a water-soluble benefit, a salt, a water-soluble organic liquid and a resin may be simultaneously added to a continuous kneader separately. Further, these components may be added to a continuous kneader after mixing. Further, it is also possible to add a resin in the process of preparing the organic pigment to prelimin to a mixture of 70% of the organic pigment and the resin. In this case, the effect of adding the resin is remarkably exhibited. The present invention 2 relates to a method for preparing a pigment composition, which comprises kneading a compound containing an organic (tetra) derivative, a ruthenium derivative or a ruthenium, an organic pigment, a water-soluble inorganic salt, and a water-soluble substance by a continuous kneader. a mixture of organic liquids, each of the above derivatives containing at least one substituent selected from the group consisting of a quinone iminomethyl group, an amine group, a phytic acid group or a (tetra) group, the continuous kneading machine comprising a drive shaft, a ring-shaped fixing plate, A rotating disk 'concentric with the disk and rotating around the axis of the drive shaft and a crushing space formed in a gap between the fixed disk and the rotating disk. 312XP/Invention Manual (Supplement y95_〇8/95114255 19 200706604 Organic used in the present invention 2 containing at least one substituent selected from the group consisting of a quinone iminomethyl group, an amine group, a sulfonic acid group or a carboxylic acid group The dye derivative is an organic dye derivative represented by the following formula (1), - P-{Xi-(Yi)k}m (1) wherein P represents an organic dye residue; Χι is a single bond or represents _ 〇_, -S-, -(3)-, -S〇2-, -, -C0NR, -SOAR^, -NRlC〇- or NRJOr, linear or branched alkylene group having 1 to 12 carbon atoms' a benzene or a triple residue substituted with an alkyl group, an amine group, a nitro group, a hydroxyl group, an alkoxy group or an atom, or a joint linking group composed of at least two of these linking groups, wherein h represents a hydrogen atom, an alkane Or a hydroxyalkyl group; 1 is a fluorenylene fluorenyl group which may be substituted by a nitro group or a halogen atom, an NR2r3, -s〇3 · M/n or a c〇〇·M/n; wherein R2 and R3 Each of them independently represents a hydrogen atom, a substituted or unsubstituted alkyl group, a substituted or unsubstituted dilute group or a substituted or unsubstituted phenyl group, or R 2 and R 3 together form a substituted or unsubstituted heterocyclic ring, the heterocyclic ring To include an additional nitrogen atom, an oxygen atom or a sulfur atom, Μ represents a hydrogen ion, a metal ion having a valence of _1 to 3 or an ammonium ion substituted with at least one alkyl group, η is a valence of hydrazine, and k is 1 or 2 An integer; m is an integer from 1 to 4. A brewing derivative containing at least one substituent selected from the group consisting of a fluorenylene sulfhydryl group, an amine group, a sulphate group or a tick acid group used in the present invention 2 Typically, it is an awake derivative represented by the following formula (2), Q-{X2-(Y2)k}m (2) wherein Q represents an alkyl group, an amine group, a nitro group, a hydroxyl group, an alkoxy group. A residue substituted with a halogen or a halogen atom; X2 is a single bond or represents -Ο-, -Co-, -SO2-, -NRi-, -CONRi-, -S〇2NR丨-, -NRiCO- or NRIS 〇2-, with 312XP/invention specification (supplement)/95-08/95114255 20 200706604 ^ Linear or branched alkylene group of 1 to 12 carbon atoms, which can be alkyl, amine, Jingji, 29 base, silk a phenyl or trisyl group substituted with a (iv) or a linking group consisting of at least two of these linking groups, wherein

Ri表不氫原子、烧基或髮烧基;γ2是可以被硝基或齒原子 取代的酞醯亞胺基甲基、一陬也、-S〇3 · Μ/η或一C00 · Μ/η ; 其中匕和R3每—個單獨表示氫原子、取代或未取代的烧 基、取代或未取代的烯基或取代或未取代的苯基,或者 R2和R3 —起形成取代或未取代的雜環,該雜環可以包含另 外的氮原子、氧原子或硫原子,M表示氫離子、化合價為 1到3的金屬離子或被至少一個烷基取代的銨離子,η是 Μ的化合價;k是1或2的整數;m是從丨到4的整數。 用在本發明2中的含有至少一個選自酞醯亞胺基甲 基、胺基、磺酸基或羧酸基的取代基的三啡衍生物典型地 是由下述式(3)代表的蒽醌衍生物, / X3— <Y3) ρ X4~ (y^ q (3) \ xs_ (Ys) r 其中R表不一讲殘基’ X3-X5中的每一個獨立地是單鍵 或表示-0-、-S-、-C0-、-S〇2-、-NRi-、-CONRi-、-S〇2NRi-、 -NLC0-或NRdO2-,具有1到12個碳原子的線性或支鏈亞 烴基,可以被烷基、胺基 '硝基、羥基、烷氧基或齒原子 取代的笨殘基、或者由至少兩個這些連接基團組成的聯合 連接基團’其中Ri表示氫原子、烧基或經烧基;γ3是可以 被硝基或鹵原子取代的酞醯亞胺基曱基、一NR2r3、 312XP/發明說明書(補件)/95-08/95114255 21 200706604 —抓1/11或一(:00._;其中1^和1^每一個單獨表示氣 原子、取代或未取代的烷基、取代或未取代的烯基或取代 或未取代的笨基,或者R3—起形成取代或未取代的 雜環,該雜環可以包含另外的氮原子、氧原子或硫原子, Μ表示氫離子、化合價為!到3的金屬離子或被至少一個 院基取代的銨離子,η是Μ的化合價;Ys每—個獨立 地具有與Y3的定義相同的定義或者表示烷基、胺基、硝Ri represents no hydrogen atom, alkyl group or calcining group; γ2 is a quinone imidomethyl group which may be substituted by a nitro group or a tooth atom, a fluorene group, -S〇3 · Μ/η or a C00 · Μ/ η ; wherein 匕 and R 3 each independently represent a hydrogen atom, a substituted or unsubstituted alkyl group, a substituted or unsubstituted alkenyl group or a substituted or unsubstituted phenyl group, or R 2 and R 3 together form a substituted or unsubstituted a heterocyclic ring which may contain an additional nitrogen atom, an oxygen atom or a sulfur atom, M represents a hydrogen ion, a metal ion having a valence of 1 to 3 or an ammonium ion substituted with at least one alkyl group, and η is a valence of hydrazine; k Is an integer of 1 or 2; m is an integer from 丨 to 4. The trimorphine derivative containing at least one substituent selected from the group consisting of a quinone iminomethyl group, an amine group, a sulfonic acid group or a carboxylic acid group used in the present invention 2 is typically represented by the following formula (3). Anthracene derivative, / X3— <Y3) ρ X4~ (y^ q (3) \ xs_ (Ys) r where R is not a residue. Each of X3-X5 is independently a single bond or Represents -0-, -S-, -C0-, -S〇2-, -NRi-, -CONRi-, -S〇2NRi-, -NLC0- or NRdO2-, having a linearity of 1 to 12 carbon atoms or a branched alkylene group, a stupid residue which may be substituted by an alkyl group, an amino group 'nitro group, a hydroxyl group, an alkoxy group or a tooth atom, or a joint linking group consisting of at least two of these linking groups' wherein Ri represents hydrogen Atom, an alkyl group or a burnt group; γ3 is a quinone imine fluorenyl group which may be substituted by a nitro group or a halogen atom, an NR2r3, 312XP/invention specification (supplement)/95-08/95114255 21 200706604 - grab 1 /11 or one (:00._; wherein 1^ and 1^ each independently represent a gas atom, a substituted or unsubstituted alkyl group, a substituted or unsubstituted alkenyl group or a substituted or unsubstituted stupid group, or R3- Form a substituted or unsubstituted heterocyclic ring The heterocyclic ring may contain an additional nitrogen atom, an oxygen atom or a sulfur atom, Μ represents a hydrogen ion, a metal ion having a valence of ! to 3 or an ammonium ion substituted by at least one of the substituents, η is the valence of hydrazine; Ys is each Independently having the same definition as Y3 or representing alkyl, amine, and nitrate

基、經基、料基、鹵原子或取代絲取代的苯基;p、q 和r每一個獨立地是1或2的整數。 用在本&明2中式⑴有機染料衍生物的有機染料的例 子包括二酮料並料染料、偶氮類染料比如偶氮染料、 重氮染料和多偶氮染料、酞青染料、蒽醌染料比如二胺基 聯恩醌、蒽素嘧啶、黃烷场、蒽嵌蕙醌、靛蕙醌、皮蒽 酮和葱酮t、啥σ丫酮染料、二„等畊染料、紫環_ (卿 染料、二萘嵌苯染料、硫散藍染料、異^朵琳染料、異吲 嗓琳酮染料、錢賴㈣、士林染料和金屬絡合染料。 式(2)蒽崎生物的蒽g昆是可以包含取代基比如由甲基或 乙基代表㈣基、胺基、硝基、歸、由甲氧基或乙氧基 代表的院氧基、或由氯代表㈣原子的蒽酿。式⑻三讲 衍生物的三畊是1,3, 5 —三畊。 本电明2中的式⑴的有機染料衍生物、式⑵的葱酿衍 生物矛式(3)的二4彡了生物是經由將特殊取代基引入到上 述有機染料、蒽醌或三畊上獲得的有機化合物。取代基的 例子包㈣醯亞胺基甲基、4-石肖基歐醯亞胺基甲基、4-312XP/發明說明書(補件)/95-〇8/95114255 22 200706604 氯酞醯亞胺基甲基、四氯酞醯亞胺基曱基、(4, 6-雙(狄酿 亞胺基曱胺基)-1,3, 5-三讲)-2-基胺基曱基、胺基曱酿 基、胺磺醯基、曱胺基、乙胺基、丙胺基、丁胺基、己胺 基、辛胺基、十二烷胺基、十八烷胺基、二曱胺基、二乙 胺基、二丁胺基、二曱胺基丙胺基、二乙胺基丙胺基、二 乙胺基乙胺基、二丁胺基丙胺基、呱啶基曱基、二曱胺基 曱基、二乙胺基曱基、二丁胺基曱基、(4, 6-雙(二乙胺基 丙胺基)-1,3,5-三讲)-2-基、(4,6-雙(二乙胺基丙胺 ®基)-1,3,5-三讲)-2-基胺基、(4-(二乙胺基丙胺基)- 6-羥基-1,3,5-三讲)-2-基胺基、二曱胺基丙胺磺醯基、二 乙胺基丙胺磺醯基、二丁胺基丙胺磺醯基、嗎啉代乙胺磺 醯基、二曱胺基丙胺羰基、4-(二乙胺基丙胺羰基)苯胺基 羰基、二甲胺基曱羰基胺曱基、二乙胺丙基胺曱基羰基胺 甲基、二丁胺丙基胺曱基羰基胺曱基、磺酸基、磺酸鈉基、 磺酸鈣基、磺酸锶基、磺酸鋇基、磺酸鋁基、4-(磺酸鋁 肇基)苯基胺甲醯基曱基、十二烷基胺基磺酸基、十八烷基 胺基磺酸基、三甲基十八烷基胺基磺酸基、二甲基二癸基 胺基磺酸基、羧酸基和2-羧酸鋁-5-硝基苯甲醯胺基曱基。 對於式(3)的三讲衍生物,除上述取代基外,取代基的例 子還包括羥基、胺基、甲氧基、乙氧基、苯氧基、4—硝基 ,苯胺基、4-苯胺基苯胺基或4-胺基苯氧基。 本發明2中的式(1)的有機染料衍生物、式(2)的蒽醌衍 生物和式(3)的三畊衍生物能夠經由公開在例如 JP-A-54-62227 、 JP-B-39-28884 、 JP-A-51-18736 、 312XP/發明說明書(補件)/95-08/95114255 23 200706604 JP-A-56-32549 、 JP-A-56-81371 、 JP-A-56-118462 、 JP-A-56-166266 、 JP-A-59-96175 、 JP-A-60-88185 、 JP-A-60-98525 、 JP-A-63-305173 、 JP-A-03-26767 和 JP-A-1 1 -1 99796中的方法製備。 本發明2中的式(1)的有機染料衍生物、式(2)的蒽醌衍 生物和式(3)的三畊衍生物的特殊例子用化合物編號顯示 如下。 化合物(1)a phenyl group substituted with a radical, a thiol group, a halogen atom or a substituted filament; each of p, q and r is independently an integer of 1 or 2. Examples of the organic dye used in the organic dye derivative of the formula (1) of the present invention include a diketone dye, an azo dye such as an azo dye, a diazo dye and a polyazo dye, an indigo dye, and an anthraquinone dye. Dyes such as diamine hydrazine, decane pyrimidine, flavane field, ruthenium ruthenium, osmium, ketone and onion ketone t, 啥σ丫 ketone dye, dioxin dye, purple ring _ ( Qing dye, perylene dye, sulfur blue dye, iso-dulin dye, isoindolinone dye, Qian Lai (four), Shilin dye and metal complex dye. (2) 蒽 生物The oxime is a ruthenium which may contain a substituent such as a methyl group or an ethyl group representing a (tetra) group, an amine group, a nitro group, a ruthenium group, a methoxy group represented by a methoxy group or an ethoxy group, or a chlorine atom representing a (tetra) atom. (8) The third ploughing of the derivative is 1, 3, 5 - three tillage. The organic dye derivative of formula (1) and the onion-brewed derivative of formula (2) of this genus 2 (2) It is an organic compound obtained by introducing a specific substituent to the above organic dye, hydrazine or three tillage. Examples of the substituent include (IV) quinone imine Methyl, 4- stone succinyl iminomethyl, 4-312XP/invention specification (supplement)/95-〇8/95114255 22 200706604 chloropurine iminomethyl, tetrachloroindenyl hydrazine Base, (4,6-bis(di-iminoimido)amino-1,3,5-trisyl)-2-ylamino fluorenyl, amine aryl, amine sulfonyl, decylamine Base, ethylamino, propylamino, butylamino, hexylamino, octylamino, dodecylamino, octadecylamino, diammonium, diethylamino, dibutylamine, dioxime Aminopropylamino, diethylaminopropylamino, diethylaminoethylamine, dibutylaminopropylamine, acridinesulfonyl, dimethylaminoindenyl, diethylaminoguanidino, dibutylamine Base group, (4,6-bis(diethylaminopropylamino)-1,3,5-trisyl)-2-yl, (4,6-bis(diethylaminopropylamine®)-1 , 3,5-three-speaking)-2-ylamino, (4-(diethylaminopropylamino)-6-hydroxy-1,3,5-tris)-2-ylamino, diamine Acetosylsulfonyl, diethylaminopropylaminesulfonyl, dibutylaminopropylaminesulfonyl, morpholinoethylaminesulfonyl, dimethylaminopropylaminecarbonyl, 4-(diethylaminopropylaminecarbonyl) Anilinocarbonyl, dimethylamino hydrazinylcarbonyl fluorenyl, diethylamine propylamine decylcarbonylamine methyl, dibutylamine propylamine decylcarbonylamine sulfhydryl, sulfonic acid group, sodium sulfonate, sulfonate Calcium acid base, sulfonate sulfonate, sulfonate sulfonate, aluminum sulfonate, 4-(sulfonate sulfonyl) phenylamine decyl fluorenyl, dodecylamino sulfonate, octadecane Amino sulfonic acid group, trimethyloctadecylamino sulfonic acid group, dimethyldidecylamino sulfonic acid group, carboxylic acid group and aluminum 2-carboxylate-5-nitrobenzamide For the three-way derivative of the formula (3), in addition to the above substituents, examples of the substituent include a hydroxyl group, an amine group, a methoxy group, an ethoxy group, a phenoxy group, a 4-nitro group, and an aniline. Base, 4-anilinoanilide or 4-aminophenoxy. The organic dye derivative of the formula (1), the anthracene derivative of the formula (2) and the tri-farm derivative of the formula (3) in the invention 2 can be disclosed, for example, in JP-A-54-62227, JP-B. -39-28884, JP-A-51-18736, 312XP/Invention Manual (Repair)/95-08/95114255 23 200706604 JP-A-56-32549, JP-A-56-81371, JP-A-56 -118462, JP-A-56-166266, JP-A-59-96175, JP-A-60-88185, JP-A-60-98525, JP-A-63-305173, JP-A-03-26767 Prepared by the method in JP-A-1 1 -1 99796. Specific examples of the organic dye derivative of the formula (1), the oxime derivative of the formula (2) and the tri-negative derivative of the formula (3) in the invention 2 are shown below by the compound number. Compound (1)

化合物(2 )Compound (2)

化合物(3)Compound (3)

312XP/發明說明書(補件)/95-08/95114255 24 200706604 化合物(4 )312XP/Invention Manual (supplement)/95-08/95114255 24 200706604 Compound (4)

化合物(7 )Compound (7)

312XP/發明說明書(補件)/95-08/95114255 25 200706604 選自:训的有機染料衍生物、式⑵的㈣衍生物和式 、啡何生物的有機化合物、有機顏料、水溶性益機 ::: !性!機液體中每一個均為本發明2的揑合:成 ’匕們可以同時獨立地添加到連續揑合機中。另 q這些組分可以在混合後添加到連續揑合機中。此外, :::能在製備有機顏料的過程中添加上述衍生物以預 ’成有機顏料和衍生物的混合物 現出衍生物的添加效果。 ‘貝者呈 ^發明的連續揑合機的操作條件不受特別限制。為了控 制有機顏料的處理量或獲得的微細有機顏料的質量,調節 揑合溫度和機械能的輸人量(主軸(傳動们21)的轉數、 原料的供應量、主軸的動力負載等)是可能的。為了有機 ,料粒子的研磨和由於它們與水溶性有機液體接觸而導 =的有機顏料粒子的生長,以及為了通過將樹脂溶解在水 浴性有機液體中而將樹脂吸收到有機顏料表面上的有效 進度,揑合溫度較佳為1Q到15(rc,特佳4G到i3(rc。 揑合溫度的升高能夠促進顏料粒子的生長速度。顏料组成 物的處理量或質量能夠通過調節揑合組成物的混合比、捏 合溫度、和機械能的輸入量(主軸(傳動軸121)的轉數、 原料的供應量、主軸的動力負載等)來控制。當揑合溫度 高於15(TC時,粒子生長是相當可觀的,以致於需要在短 時間内進行揑合。然而,在該情況下,粒子均句化的時間 變得較短’考慮到質量’這不是可取的。揑合開始後,根 據需要進行加熱或冷卻1外’通過在連續揑合機的中間 312XP/發明說明書(補件)/95-08/95114255 200706604 位置設置原料人口以及在連續揑合步驟中添加樹脂、衍生 物或水溶性有機液體’改變揑合組成物的混合比是可能 的:通過串連連接多個連續揑合機、並且不同地調整各個 連續揑=機的操作條件來調節整個揑合條件也是可能的。 根據常用方法處理揑合後的顏料組成物。也就是說,用 水或無機酸水溶液處理揑合組成物,然後㈣並用水洗 條’從而去除水溶性無機鹽和水溶性有機液體並分離顏料 組成物。可以直接使用潮濕狀態的顏料組成物。此外,也 可以使用通過乾燥和粉碎獲得的粉末態的顏料組成物。根 據而要’揑合後可以添加樹脂、表面活性劑和/或其他添 微細有機顏料的平均原始粒徑會根據細碎處理的 和有機顏料的種類進行變化。通過適當調整條件可以 始粒徑任意地控制在約10到50〇nm的範圍内。 ’、312XP/Invention Manual (Supplement)/95-08/95114255 25 200706604 From: Organic dye derivatives, (4) derivatives and formulas, organic compounds, organic pigments, water-soluble benefits: :: ! Sex! Each of the machine liquids is the kneading of the present invention 2: they can be simultaneously independently added to the continuous kneader. Alternatively, these components can be added to the continuous kneader after mixing. Further, ::: The above derivative can be added in the course of preparing an organic pigment to pre-form a mixture of an organic pigment and a derivative to exhibit an additive effect. The operating conditions of the continuous kneader invented by the presenter are not particularly limited. In order to control the amount of processing of the organic pigment or the quality of the obtained fine organic pigment, it is possible to adjust the pinch temperature and the amount of mechanical energy input (the number of revolutions of the spindle (driver 21), the supply of the raw material, the power load of the spindle, etc.) of. For the organic, the grinding of the material particles and the growth of the organic pigment particles guided by their contact with the water-soluble organic liquid, and the effective progress of absorbing the resin onto the surface of the organic pigment by dissolving the resin in the water-bath organic liquid The kneading temperature is preferably from 1Q to 15 (rc, particularly preferably from 4G to i3 (rc.) The increase in the kneading temperature can promote the growth rate of the pigment particles. The treatment amount or mass of the pigment composition can be adjusted by adjusting the mixing ratio of the kneaded composition. , the kneading temperature, and the input of mechanical energy (the number of revolutions of the main shaft (the drive shaft 121), the supply of the raw material, the dynamic load of the main shaft, etc.). When the kneading temperature is higher than 15 (TC, the particle growth is considerable. Therefore, it is necessary to perform kneading in a short time. However, in this case, the time for particle homogenization becomes shorter, which is not preferable in consideration of quality. After the kneading starts, heating or cooling is performed as needed. External 'by setting the raw material population in the middle of the continuous kneading machine 312XP / invention manual (supplement) / 95-08/95114255 200706604 and in the continuous kneading step It is possible to change the mixing ratio of the kneaded composition by adding a resin, a derivative or a water-soluble organic liquid: the entire kneading condition is adjusted by connecting a plurality of continuous kneaders in series, and adjusting the operating conditions of the respective continuous kneaders differently It is possible to treat the kneaded pigment composition according to a usual method, that is, to treat the kneaded composition with water or an aqueous solution of an inorganic acid, and then (4) to wash the strip with water to remove the water-soluble inorganic salt and the water-soluble organic liquid and separate the pigment composition. The pigment composition in a wet state can be used as it is. In addition, a powdery pigment composition obtained by drying and pulverization can also be used. It is also possible to add a resin, a surfactant, and/or other fine organic pigments after kneading. The average primary particle diameter varies depending on the type of the finely divided and organic pigments. The particle size can be arbitrarily controlled to be in the range of about 10 to 50 〇 nm by appropriately adjusting the conditions.

在本發明的顏料組成物中,藉助於特殊的連續 少量的能量製備極細顏料粒子。為了使顏料組成物結持 裱細顏料粒子的情形下能夠分散在油墨或塗料中 步驟中通過由於添加樹脂或衍生物而利用樹脂 Z 塗覆顏料粒子,減少顏料粒子的相互團聚,同時保持 碎顏料粒子。本發明的賴組成物適用於要求高透明度的田 應用。因此’本發明的顏料組成物在如凹印油墨、喷黑油 墨和滤色器的應用中表現出了特別優異的質量。此外tl ^如謬印油墨、塗料、塑膠著色和彩色調色劑的^ 表現出了優異的質量。例如,當製備凹印油墨時^用的 312XP/發明說明書(補件)/95_〇8/95114255 ιη 200706604In the pigment composition of the present invention, extremely fine pigment particles are prepared by means of a special continuous small amount of energy. In order to allow the pigment composition to be adhered to the fine pigment particles, it is possible to disperse in the ink or coating step by coating the pigment particles with the resin Z by adding a resin or a derivative, thereby reducing mutual agglomeration of the pigment particles while maintaining the crushed pigment particle. The composition of the present invention is suitable for field applications requiring high transparency. Therefore, the pigment composition of the present invention exhibits particularly excellent quality in applications such as gravure inks, black ink jets, and color filters. In addition, tl ^ such as enamel printing ink, paint, plastic coloring and color toners ^ showed excellent quality. For example, when preparing a gravure ink, the 312XP/invention specification (supplement)/95_〇8/95114255 ιη 200706604

載色劑由樹脂和溶劑組成。載色劑不受特別限制而且可以 包含助劑或增I顏料。樹脂的例子包括松香、木蒸松香、 =爾油松香、石灰松香、松香酯、馬來酸樹脂、聚醯胺樹 脂、乙烯基樹脂、硝酸纖維素、乙酸纖維素、乙基纖維素、 氯化橡膠、環化橡膠、乙烯—醋酸乙烯酯共聚樹脂、尿烷 樹脂、聚酯樹脂、醇酸樹脂、丙烯酸樹脂、黑瀝青、達馬 才'f月曰触膠含有上述樹脂的樹脂混合物、通過使任何二 種上述樹脂混合物和上述樹脂溶解在水中獲得的水溶性 树脂、以及乳化樹脂。溶劑例如,包括烴、醇、酮、醚醇、 醚、酯和水。特別是,當使用纖維素類樹脂時,能夠獲得 具有良好透明度、高光澤度和高清晰度的高質量凹印油 墨。此外,通過使用分散裝置比如溶解器、高速混合器、 均勻混合器、揑合機、沖洗器、輥式破碎機、砂磨機或磨 碎機,使顏料組成物極好地與載色劑混合或將其分散在載 色劑中。 • 由本發明3提供的用於濾色器的著色組成物是包含由 透明樹脂、其先質或其混合物組成的顏料載體和顏料的用 於濾色器的著色組成物,該著色組成物的特徵在於該顏料 包含用連續揑合機揑合包含有機顏料、水溶性無機鹽和水 /奋性有機液體的混合物獲得的微細有機顏料,上述連續揑 -合機包括傳動軸、環形固定盤、與固定盤同心而且整個繞 傳動軸的軸旋轉的旋轉盤,以及在固定盤和旋轉盤之間的 間隙中形成的粉碎空間。 此外,本發明3的濾色器的特徵在於該濾色器包括由本 312XP/發明說明書(補件)/95-08/95114255 28 200706604 發明的著色組成物形成㈣色器片。 10揑合處理的 液體以及任選 下文中有時稱 然後,將詳細說明即將經受連續揑合機 含有有機_、水溶性無機鹽和水溶性 含有的樹脂和/或顏料衍生物的混合物’ 作「揑合組成物」)。 中的有機顏料選自用於遽色器的已知有 =徑Γ〇1顏:可以被單獨使用或聯… 時,^以將m、G.5 A m的有機顏料用作該有機顏料 ^了㈣有機顏料細細地粉碎成平均原始粒徑為〇 〇1 二的極細粒子而且呈現出特別高的對比度,所以 j =這種有機顏料。作為有機顏料,還可以使用狀態 不曰因匕的合成而改變的粗有機顏料,即,可以使用(a) 平均原始粒徑約為1G到2叫m的大粒子或⑻平均原始 粒徑為G.Glp或以下的極細粒子的極強成糰粒子(聚集 在下面用色度指數說明可用於本發明3的有機顏料的 特殊例子。 對於用於形成紅色濾色器片的紅色著色組成物,可以使 用紅色顏料如C· I·顏料紅7、9、14、41、48 :1、48 · 2、 48:3、48:4、81 Η、81:2、81:3、97、122、123、146、 149 、 168 、 177 、 178 、 180 、 184 、 185 、 187 、 192 、 200 、 202 、 208 、 210 、 215 、 216 、 217 、 220 、 223 、 224 、 226 、 227、228、240、246、254、255、264 和 272。在紅色顏 料組成物中,可以另外使用黃色顏料和/或橙色顏料。 312ΧΡ/發明說明書(補件)/95-08/95114255 29 200706604 對於用於形成黃色濾色器片的黃色著色組成物,可以使 用黃色顏料如c· I.顏料黃1、2、3、4、5、6、10、12、 13、14、15、16、17、18、20、24、3卜 32、34、35、35:1、 36、36:;1、37、37:;1、40、42、43、53、55、60、6卜 62、 63、65、73、74、77、81、83、86、93、94、95、97、98、 100、1(Π、104、106、108、109、110、113、114、115、 116、117、118、119、120、123、125、126、127、128、 129、137、138、139、147、148、150、151、152、153、 • 154、155、156、161、162、164、166、167、168、169、 170、171、172、173、174、175、176、177、179、180、 18卜 182、185、187、188、193、194 和 199。 對於用於形成橙色濾色器片的撥色著色組成物,可以使 用橙色顏料如C· I·顏料橙36、43、51、55、59和61。 對於用於形成綠色濾色器片的綠色著色組成物,可以使 用綠色顏料如C· I·顏料綠7、1〇、36和37。在該綠色 籲著色組成物中,可以另外使用黃色顏料。 對於用於形成藍色濾色器片的藍色著色組成物,可以使 用藍色顏料如C· L顏料藍15、15:1、15··2、15:3、15:4、 15· 6、16、22、60和64。在該藍色著色組成物中,可以 另外使用紫色顏料如c· I·彥貝料紫1、19、23、27、29、 30 、 32 、 37 、 40 、 42 和 50 。 對於用於形成青色濾色器片的青色著色組成物,可以使 用藍色顏料如ρ τ & ^ 4 c ^ Λ L· 1 ·顏料藍 15 :1、15 : 2、15 : 4、15 : 3、 15 : 6、16 和 81 〇 312ΧΡ/____5·0 祕 114255 200706604 對於用於形成品紅色濾色器片的品紅色著色組成物,可 以使用紫色顏料和紅色顏料如c·丨·顏料紫丨和19和c. I·顏料紅Red 144、146、177、169和81。在該品紅色 著色組成物中,可以另外使用黃色顏料。 當揑合有機顏料、水溶性無機鹽和水溶性有機液體的混 合物時,為了防止有機顏料的晶體生長或晶體轉化,可以 添加通過將鹼性或酸性取代基或酞醯亞胺基甲基引入到 有機顏料、蒽醌、吖啶酮或三畊中獲得的衍生物。尤其是, 較佳添加通過將鹼性或酸性取代基或酞醯亞胺基甲基引 入到有機顏料中獲得的顏料衍生物。作為鹼性取代基,可 以使用由以下式(4)到(7)代表的取代基。酸性取代基典型 地為確酸基或叛基。 基質結構與細碎的有機顏料相同的顏料衍生物較佳作 為該顏料衍生物。也可以使用基質結構與細碎的有機顏料 不同的顏料衍生物。 在揑合組成物中,每丨重量份有機顏料使用的顏料衍生 物的量較佳為0.001重量份到〇. 3重量份。當顏料衍生物 的量小於0.001重量份時,難以達到添加效果。當顏料衍 生物的里大於〇· 3重量份時,不能達到與添加量相應的效 果,另外,使獲得的微細有機顏料成為顏料和顏料衍生物 的混合物。在該情況下,作為單一物質的有機顏料在物理 性質上的差異變得較大,以致於有時通過使用含有這種微 細有機顏料的著色組成物形成的濾色器會在實際質量上 存在問題。 、”、 312XP/發明麵書(補件)/95-08/95114255 31 200706604The vehicle is composed of a resin and a solvent. The vehicle is not particularly limited and may contain an auxiliary or an I-increasing pigment. Examples of the resin include rosin, wood steamed rosin, er oil rosin, lime rosin, rosin ester, maleic acid resin, polyamide resin, vinyl resin, nitrocellulose, cellulose acetate, ethyl cellulose, chlorination Rubber, cyclized rubber, ethylene-vinyl acetate copolymer resin, urethane resin, polyester resin, alkyd resin, acrylic resin, black asphalt, Damascus's resin mixture containing the above resin, Any two of the above resin mixtures and the water-soluble resin obtained by dissolving the above resin in water, and an emulsified resin. Solvents include, for example, hydrocarbons, alcohols, ketones, ether alcohols, ethers, esters, and water. In particular, when a cellulose-based resin is used, a high-quality gravure ink having good transparency, high gloss, and high definition can be obtained. Further, by using a dispersing device such as a dissolver, a high-speed mixer, a homomixer, a kneader, a rinser, a roll crusher, a sand mill or an attritor, the pigment composition is excellently mixed with the vehicle or It is dispersed in the vehicle. • The coloring composition for a color filter provided by the present invention 3 is a coloring composition for a color filter comprising a pigment carrier and a pigment composed of a transparent resin, a precursor thereof or a mixture thereof, characteristics of the coloring composition The pigment comprises a fine organic pigment obtained by kneading a mixture comprising an organic pigment, a water-soluble inorganic salt and a water/exciting organic liquid by a continuous kneader, the continuous kneading machine comprising a drive shaft, a ring-shaped fixing plate, and a concentric disk Further, the entire rotary disk that rotates around the axis of the drive shaft, and the pulverizing space formed in the gap between the fixed disk and the rotary disk. Further, the color filter of the present invention 3 is characterized in that the color filter comprises a (four) color former sheet formed by the coloring composition invented by the present invention 312XP/invention specification (supplement)/95-08/95114255 28 200706604. 10 kneading treated liquid and optionally hereinafter sometimes referred to as a "kneading composition" which will be subjected to a continuous kneader containing a mixture of an organic _, a water-soluble inorganic salt and a water-soluble resin and/or a pigment derivative ")"). The organic pigment in the coloring agent is selected from the group of known pigments for use in a coloring device: when it can be used alone or in combination, the organic pigment of m, G.5 A m is used as the organic pigment. (4) The organic pigment is finely pulverized into extremely fine particles having an average primary particle diameter of 〇〇1 and exhibits a particularly high contrast, so j = such an organic pigment. As the organic pigment, it is also possible to use a crude organic pigment whose state does not change due to the synthesis of ruthenium, that is, (a) a large particle having an average primary particle diameter of about 1 G to 2 m or (8) an average primary particle diameter of G can be used. Very strong agglomerated particles of very fine particles of Glp or below (aggregated below, a specific example of an organic pigment which can be used in the present invention 3 is illustrated by a chromaticity index. For the red colored composition for forming a red color filter sheet, Use red pigments such as C·I·Pigment Red 7, 9, 14, 41, 48:1, 48 · 2, 48:3, 48:4, 81 Η, 81:2, 81:3, 97, 122, 123 , 146, 149, 168, 177, 178, 180, 184, 185, 187, 192, 200, 202, 208, 210, 215, 216, 217, 220, 223, 224, 226, 227, 228, 240, 246 254, 255, 264 and 272. In the red pigment composition, yellow pigments and/or orange pigments may additionally be used. 312 ΧΡ / invention specification (supplement) / 95-08/95114255 29 200706604 for forming yellow color filters Yellow coloring composition of the tablet, yellow pigment such as c·I. pigment yellow can be used 1, 2, 3, 4, 5, 6, 10, 12, 13, 14, 15, 16, 17, 18, 20, 24, 3, 32, 34, 35, 35:1, 36, 36:;1 , 37, 37:; 1, 40, 42, 43, 53, 55, 60, 6 Bu 62, 63, 65, 73, 74, 77, 81, 83, 86, 93, 94, 95, 97, 98, 100, 1 (Π, 104, 106, 108, 109, 110, 113, 114, 115, 116, 117, 118, 119, 120, 123, 125, 126, 127, 128, 129, 137, 138, 139, 147, 148, 150, 151, 152, 153, • 154, 155, 156, 161, 162, 164, 166, 167, 168, 169, 170, 171, 172, 173, 174, 175, 176, 177, 179 180, 18, 182, 185, 187, 188, 193, 194, and 199. For the coloring and coloring composition for forming the orange color filter sheet, an orange pigment such as C·I·Pigment Orange 36, 43 may be used. 51, 55, 59, and 61. For the green coloring composition for forming a green color filter sheet, green pigments such as C·I·Pigment Green 7, 1, 36, 36, and 37 can be used. In addition, a yellow pigment may be additionally used. For the blue coloring composition for forming the blue color filter sheet, a blue pigment such as C·L Pigment Blue 15, 15:1, 15·2, 15:3, 15:4, 15·6 can be used. 16, 22, 60 and 64. In the blue coloring composition, a purple pigment such as c·I·Yanbeizi 1, 19, 23, 27, 29, 30, 32, 37, 40, 42 and 50 may be additionally used. For the cyan coloring composition for forming a cyan color filter sheet, a blue pigment such as ρ τ & ^ 4 c ^ Λ L· 1 · Pigment Blue 15 : 1, 15 : 2, 15 : 4, 15 can be used: 3, 15 : 6, 16 and 81 〇 312 ΧΡ / ____5 · 0 Secret 114255 200706604 For the magenta colored composition used to form the magenta color filter sheet, purple pigment and red pigment such as c·丨·pigment purpura can be used. And 19 and c. I·Pigment Red Red 144, 146, 177, 169 and 81. In the magenta colored composition, a yellow pigment may be additionally used. When kneading a mixture of an organic pigment, a water-soluble inorganic salt, and a water-soluble organic liquid, in order to prevent crystal growth or crystal transformation of the organic pigment, it may be added by introducing a basic or acidic substituent or a guanidinomethyl group to the organic a derivative obtained by pigment, hydrazine, acridone or tricot. In particular, a pigment derivative obtained by introducing a basic or acidic substituent or a quinone iminomethyl group into an organic pigment is preferably added. As the basic substituent, a substituent represented by the following formulas (4) to (7) can be used. The acidic substituent is typically an acid group or a thiol group. A pigment derivative having the same matrix structure as the finely divided organic pigment is preferred as the pigment derivative. It is also possible to use a pigment derivative in which the matrix structure is different from the finely divided organic pigment. The amount of the pigment derivative used per part by weight of the organic pigment in the kneaded composition is preferably from 0.001 part by weight to 0.3 parts by weight. When the amount of the pigment derivative is less than 0.001 part by weight, it is difficult to achieve an additive effect. When the amount of the pigment derivative is more than 〇·3 parts by weight, the effect corresponding to the added amount cannot be attained, and in addition, the obtained fine organic pigment is made into a mixture of the pigment and the pigment derivative. In this case, the difference in physical properties of the organic pigment as a single substance becomes large, so that sometimes a color filter formed by using a colored composition containing such a fine organic pigment may have problems in actual quality. . ,", 312XP / invention book (supplement) / 95-08/95114255 31 200706604

在式(4)到(7)中,x 表示一s〇2—、一c〇一、一CH2NHC〇CH2一、 一CH2—或單鍵;n表示1到1〇的整數;1和R2每一個獨立 地表示具有1到3 6個碳原子的取代或未取代的烧基、具 有2到36個碳原子的取代或未取代的烯基或取代或未取 代的笨基、或Ri和R2 一起形成取代或未取代的雜環,該 雜環還可以含有氮原子、氧原子或硫原子;R3表示具有i 到3 6個奴原子的取代或未取代的烧基、具有2到3 6個石炭 原子的取代或未取代的烯基或取代或未取代的苯基;r4、 Rs、Re和R?每一個獨立地表示氢原子、具有.丨到36個石炭 原子的取代或未取代的燒基、具有2到36個碳原子的取 代或未取代的烯基或取代或未取代的笨基;γ表示 -NRs-Z-NR9-或單鍵,其中R8和I每一個獨立地表示氮原 312XP/發明說明書(補件)/95-08/95114255 32 200706604 子、具有1到36個碳原子的取代或未取代的烷基、具有 2到36個碳原子的取代或未取代的烯基或取代或未取代 的本基,Z表示具有1到36個碳原子的取代或未取代的 烧撐基、具有2到36個碳原子的取代或未取代的烯撐基 或取代或未取代的苯撐基;R表示由式(8)代表的取代基,In the formulae (4) to (7), x represents an s〇2—, a c〇1, a CH2NHC〇CH2, a CH2— or a single bond; n represents an integer of 1 to 1〇; 1 and R2 per a substituted or unsubstituted alkyl group having 1 to 36 carbon atoms, a substituted or unsubstituted alkenyl group having 2 to 36 carbon atoms or a substituted or unsubstituted stupid group, or Ri and R2 together a substituted or unsubstituted heterocyclic ring may be formed, which may also contain a nitrogen atom, an oxygen atom or a sulfur atom; R3 represents a substituted or unsubstituted alkyl group having from i to 36 slave atoms, and has 2 to 36 carbon charcoal a substituted or unsubstituted alkenyl group or a substituted or unsubstituted phenyl group; each of r4, Rs, Re and R? independently represents a hydrogen atom, a substituted or unsubstituted alkyl group having from 丨 to 36 carbon atoms. a substituted or unsubstituted alkenyl group having 2 to 36 carbon atoms or a substituted or unsubstituted stupid group; γ represents a -NRs-Z-NR9- or a single bond, wherein each of R8 and I independently represents a nitrogen source 312XP /Invention Manual (Supplement)/95-08/95114255 32 200706604 Substituted, substituted or unsubstituted alkyl group having 1 to 36 carbon atoms, having 2 to 36 A substituted or unsubstituted alkenyl group or a substituted or unsubstituted base of the atom, Z represents a substituted or unsubstituted alkylene group having 1 to 36 carbon atoms, a substituted or unsubstituted having 2 to 36 carbon atoms An olefinic group or a substituted or unsubstituted phenylene group; R represents a substituent represented by the formula (8),

其中n、Ri和R2如上定義,或是由式(9)代表的取代基,Wherein n, Ri and R2 are as defined above, or a substituent represented by the formula (9),

C»-CH (9) 其中R3到R?如上定義;Q表示羥基、烷氧基、由上式(8) 代表的取代基或由上式(9)代表的取代基。 構成顏料衍生物的有機顏料的例子包括二酮π比洛並U比 ⑩咯染料;偶氮染料如偶氮;重氮或多偶氮染料;酞青染料; 蒽酉昆染料比如二胺基聯蒽i昆、蒽素^密咬、黃士 g同、蒽欲慧 醒、散蒽酿、皮蒽酮或蒽酮紫;π奎吖g同染料;二崎0井染料; 茈酮染料;二萘嵌苯染料;硫敕藍染料;異吲哚琳染料; 〃異吲哚啉酮染料;喹諾酞酮染料;士林染料和金屬絡合染 ,料。此外,可以使用前面所述的用在揑合組成物中的顏料。 分別構成蒽醌衍生物和吖啶酮衍生物的蒽醌和吖啶酮 是各自分別可以具有取代基、比如由曱基或乙基代表的烷 基、胺基、硝基、羥基、由甲氧基或乙氧基代表的烷氧基、 312XP/發明說明書(補件)/95-08/95114255 33 200706604 或由氯代表的鹵的蒽酿和吖咬酮。 構成三畊衍生物的三畊是可以具有以下取代基的 • 1,3, 5-三畊,比如由曱基或乙基代表的烷基;胺基或由二 , 曱胺基、二乙胺基或二丁胺基代表的烷胺基;硝基、羥基、 由甲氧基、乙氧基或丁氧基代表的烷氧基;由氯代表的鹵 素、可以被曱基、曱氧基、胺基、二甲胺基或羥基取代的 苯基;或可以被曱基、乙基、曱氧基、乙氧基、胺基、二 曱胺基、二乙胺基、硝基或羥基取代的苯胺基。 各自具有鹼性取代基的顏料衍生物、蒽醌衍生物和吖啶 酮衍生物能夠通過各種合成路線合成。例如,它們可以通 過下述方式獲得:將由下式(1〇)到(13)任一代表的取代基 引入到有機顏料、蒽醌或吖啶酮中,使該取代基與能夠與 上述取代基反應的胺組分反應,以便形成由式到 任何一個代表的取代基。胺組分的例子包括N,N—二曱胺 基丙胺、N-甲基呱畊、二乙胺和4-[4-羥基-6-[3-(二丁 ⑩胺基)丙胺基]-1,3, 5-三畊基-2-基胺基]苯胺。C»-CH (9) wherein R3 to R? are as defined above; Q represents a hydroxyl group, an alkoxy group, a substituent represented by the above formula (8) or a substituent represented by the above formula (9). Examples of the organic pigment constituting the pigment derivative include a diketone π pylorium and U ratio 10 azole dye; an azo dye such as azo; a diazo or polyazo dye; an indigo dye; a quinone dye such as a diamine group.蒽i Kun, 蒽素^密咬, 黄士g同, 蒽欲慧醒, 散蒽, 蒽 蒽 蒽 or 蒽 紫 ; ;; π 奎 吖 g with dye; 崎 0 0 well dye; 茈 ketone dye; Naphthalene dye; thioindigo dye; isophthalocyanine dye; 〃 isoindolinone dye; quinolone dye; Shilin dye and metal complex dye, material. Further, the pigment used in the kneading composition described above can be used. The anthracene and acridone which respectively constitute an anthracene derivative and an acridone derivative are each an alkyl group, an amine group, a nitro group, a hydroxyl group, and a methoxy group which may each have a substituent such as a mercapto group or an ethyl group. Alkoxy group represented by a ethoxy group or ethoxy group, 312XP / invention specification (supplement) / 95-08/95114255 33 200706604 or a brewed and bitten ketone of a halogen represented by chlorine. The three-ploughed cultivating three-cultivated derivative is a 1,3,5-three-till, such as an alkyl group represented by a mercapto group or an ethyl group; an amine group or a di-anthracene group or a diethylamine. An alkylamino group represented by a benzyl or dibutylamino group; a nitro group, a hydroxyl group, an alkoxy group represented by a methoxy group, an ethoxy group or a butoxy group; a halogen represented by chlorine, which may be a thiol group, a decyloxy group, Amino, dimethylamino or hydroxy substituted phenyl; or may be substituted by fluorenyl, ethyl, decyloxy, ethoxy, amine, dimethylamino, diethylamino, nitro or hydroxy Anilino group. The pigment derivative, the anthracene derivative and the acridone derivative each having a basic substituent can be synthesized by various synthetic routes. For example, they can be obtained by introducing a substituent represented by any one of the following formulas (1〇) to (13) into an organic pigment, hydrazine or acridone such that the substituent and the above substituent are capable of The amine component of the reaction is reacted to form a substituent represented by the formula to any one of them. Examples of the amine component include N,N-diguanamine propylamine, N-methyl hydrazine, diethylamine, and 4-[4-hydroxy-6-[3-(dibutyl10amino)propylamino]- 1,3,5-trihydro-yl-2-ylamino]aniline.

(10) (11) (12) (13)(10) (11) (12) (13)

- CH2NHCOCH2CI- CH2NHCOCH2CI

- CH2CI 在由式(10)到(13)任一代表的取代基與上述胺組分的 反應中,能夠同時存在由式(1 〇)到(13)任一取代基的水解 部为形成的物貝和用經基取代氯原子形成的物質。在該情 況下,式(10)的取代基成為磺酸基而式(11)的取代基成為 312XP/發明說明書(補件)/95-08/95114255 34 200706604 羧酸基、。它們每一個均可以為游離酸。此外,它們每一個 均I以為具有化合價為1到3的金屬或上述單胺的鹽。 田"亥有機顏料是偶氮顏料時,通過預先將由式(4)到(7) 任一代表的取代基引入到重氮組分或偶合組分中,然後進 行偶口反應可以製備具有驗性基的偶氮顏料衍生物。 此外,具有特殊鹼性基團的三讲衍生物可以豸過各種合 f路線獲得。例如,它可以通過使作為起始原料的氰尿i 乳的至^ -個氯與胺組分反應,然後使氰尿醯氯的殘餘 ”胺知等反應來合成,上述與胺組分的反應形成、气 甲基α瓜畊。 下面說明了具有鹼性取代基的衍生物的特殊例子 所述衍生物不受這些例子的 ^ “、、而 使用或聯合使用。 做早镯 312XP/發明說明書(補件)/95-08/95114255 200706604 衍生物1- CH2CI In the reaction of the substituent represented by any one of the formulae (10) to (13) with the above-mentioned amine component, a hydrolyzable moiety derived from any of the substituents of the formula (1 〇) to (13) can be simultaneously formed. A substance formed by replacing a chlorine atom with a thiol group. In this case, the substituent of the formula (10) becomes a sulfonic acid group and the substituent of the formula (11) becomes a carboxylic acid group of 312XP/invention specification (supplement)/95-08/95114255 34 200706604. Each of them can be a free acid. Further, each of them is considered to have a metal having a valence of 1 to 3 or a salt of the above monoamine. When the organic pigment is an azo pigment, it can be prepared by introducing a substituent represented by any one of the formulas (4) to (7) into the diazo component or the coupling component in advance, and then performing the incident reaction. Azo pigment derivatives of the group. In addition, three-speaking derivatives with specific basic groups can be obtained by various routes. For example, it can be synthesized by reacting the chlorine of the cyanuric i-milk as a starting material with an amine component, and then reacting the residual "amine" of cyanuric chloride, which reacts with the amine component. Formation, gas methylation, and melon cultivation. Specific examples of derivatives having a basic substituent are described below. The derivatives are not used in the examples, or used in combination. Do the early bracelet 312XP / invention manual (supplement) / 95-08/95114255 200706604 derivative 1

312XP/發明說明書(補件)/95-08/95114255 36 200706604312XP / invention manual (supplement) / 95-08/95114255 36 200706604

衍生物5Derivative 5

衍生物9Derivative 9

312XP/發明說明書(補件)/95-08/95114255 37 200706604312XP/Invention Manual (supplement)/95-08/95114255 37 200706604

衍生物10Derivative 10

C2H5C2H5

[(H2C)2HN02S 312XP/發明說明書(補件)/95-08/95114255 200706604 衍生物15[(H2C)2HN02S 312XP/Invention Manual (supplement)/95-08/95114255 200706604 Derivative 15

衍生物16 4(iI2C>2HN〇2S.Derivative 16 4 (iI2C>2HN〇2S.

I|fa=N~^~^~S02NH(CH2h、 H3COCHCOCHN—/ Vn^COCHCOOh ^H5 衍生物1] c2h{ (H2Q]HN〇iS—/1 h3c〇chcoghn^ V-^racomcocHj Cl 衍生物18I|fa=N~^~^~S02NH(CH2h, H3COCHCOCHN-/Vn^COCHCOOh ^H5 derivative 1] c2h{ (H2Q]HN〇iS—/1 h3c〇chcoghn^ V-^racomcocHj Cl derivative 18

39 312XP/發明說明書(補件)/95-08/95114255 200706604 衍生物2039 312XP/Invention Manual (supplement)/95-08/95114255 200706604 Derivative 20

衍生物22Derivative 22

312XP/發明說明書(補件)/95-08/95114255 40 200706604 衍生物25312XP/Invention Manual (supplement)/95-08/95114255 40 200706604 Derivative 25

衍生物27Derivative 27

312XP/發明說明書(補件)/95-08/95114255 41 200706604 衍生物29312XP/Invention Manual (supplement)/95-08/95114255 41 200706604 Derivative 29

312XP/發明說明書(補件)/95-08/95114255 42 200706604312XP/Invention Manual (supplement)/95-08/95114255 42 200706604

衍生物32Derivative 32

312XP/發明說明書(補件)/95-08/95114255 43 200706604 衍生物37312XP/Invention Manual (supplement)/95-08/95114255 43 200706604 Derivative 37

C2H5C2H5

312XP/發明說明書(補件)/95-08/95114255 44 200706604 衍生物41312XP/Invention Manual (supplement)/95-08/95114255 44 200706604 Derivative 41

C\r-pg \ /4C\r-pg \ /4

Cu-pc ;銅酜青殘基 衍生物43Cu-pc; copper indigo residue derivative 43

312XP/發明說明書(補件)/95-08/95114255 45 200706604312XP/Invention Manual (supplement)/95-08/95114255 45 200706604

衍生物44Derivative 44

312XP/發明說明書(補件)/95-08/95114255 46 200706604 衍生物47312XP/Invention Manual (supplement)/95-08/95114255 46 200706604 Derivative 47

eu-pc ;銅欧青殘基 衍生物49Eu-pc; copper eucalyptus residue derivative 49

衍生物50Derivative 50

Cu-pc ;銅酞青殘基 312XP/發明說明書(補件)/95-〇8/95114255 47 200706604 然後#,將說明由本發明提供的用於濾色器的著色組成 物,該著色組成物含有由此獲得的微細有機顏料和顏 • 體。 將微細有機顏料分散在包含於本發明3著色組成物中 的顏料載體中。該顏料載體由透明樹脂、它的先質或它們 的此δ物組成。違透明樹脂在4〇〇到7〇〇nm的整個可見波 長中呈現出較佳80%或更多,更佳95%或更多的透光 _率。該透明樹脂包括熱塑性樹脂、熱固性樹脂和活性能量 (active energy)束可固化樹脂。它的先質包括每個均通 過活性能量束照射進行固化並由此製備透明樹脂的單體 和低聚物。這些可以單獨使用或聯合使用。 在著色組成物中,每100重量份的顏料可以使用3〇到 700重量份,較佳6〇到450重量份的顏料載體。當將透 明樹脂和其先質的混合物用作顏料載體時,在著色組成物 中’每100重量份的顏料可以使用20到400重量份,較 籲佳50到250重量份的透明樹脂。此外,在著色組成物中, 每100重量份的顏料可以使用1〇到300重量份,較佳1〇 到200重量份的透明樹脂的先質。 熱塑性樹脂的例子包括丁醛樹脂、苯乙烯—馬來酸共聚 物、氯化聚乙烯、氯化聚丙烯、聚氯乙烯、氣乙烯-醋酸 ^ 乙烯酯共聚物、聚醋酸乙烯酯、聚胺酯樹脂、聚酯樹脂、 丙烯酸樹脂、醇酸樹脂、聚苯乙烯樹脂、聚醯胺樹脂、橡 膠樹脂、環化橡膠樹脂、纖維素、聚乙烯(HDPE和LDPE)、 聚丁二烯和聚醯亞胺樹脂。熱固性樹脂的例子包括環氧樹 312XP/發明說明書(補件)/95-08/95114255 48 200706604 脂、苯代三聚氰胺樹脂、松香改性的馬來酸樹脂、松香改 性的富馬酸樹脂、二聚氰胺樹脂、尿素樹脂和酚醛樹脂。 •活性能量束可固化樹脂的例子包括··通過藉助於具有反 -應性取代基比如異氰酸酯基、醛基或環氧基的(曱基)丙烯 酸化合物或肉桂酸和上述聚合物之間的反應、將光致交聯 基團比如(甲基)丙烯醯基或苯乙烯基引入到具有反應性 取代基比如輕基、.基或胺基的聚合物中來進行製備的樹 脂,通過含有酸酐的線性聚合物如苯乙烯—馬來酸酐共聚 物或α-烯-馬來酸酐共聚物與具有羥基的(甲基)丙烯酸 化合物如羥烷基(甲基)丙烯酸酯的半酯化來進行製備的 樹脂。 作為透明樹脂的先質的單體和低聚物的例子包括各種 丙烯酸酯和甲基丙烯酸酯如(曱基)丙烯酸曱酯、(曱基) 丙烯酸乙酯、(曱基)丙烯酸2-羥乙基酯、(曱基)丙烯酸 2-羥丙基酯、(曱基)丙烯酸環己酯、(甲基)丙烯酸沒一羧 鲁乙基酉曰、t乙一醇一(曱基)丙烯酸酯、1,6-己二醇二(曱 基)丙烯酸酯、三伸乙甘醇二(甲基)丙烯酸酯、三伸丙二 醇二(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、 三(甲基)丙烯酸季戊四醇酯、丨,6—己二醇二環氧甘油醚二 (甲基)丙烯酸酯、雙酚A二環氧甘油醚二(甲基)丙烯酸 酉曰、新戊一醇二環氧甘油醚二(甲基)丙烯酸酯、六(甲基) 丙烯酸二季戊四醇酯、(甲基)丙烯酸三環癸烯酯、酯丙烯 酸酯、羥甲基化密胺的(甲基)丙烯酸酯、環氧(甲基)丙烯 酸酯和丙烯酸胺基甲酸酯;(甲基)丙烯酸、苯乙烯、醋酸 312XP/發明說明書(補件)/95-08/95114255 49 200706604 乙烯s曰、羥乙基乙烯醚、乙二醇二乙烯醚、季戊四醇三乙 烯醚、(甲基)丙稀醯胺、N—經甲基(甲基)丙烯醯胺、N一 乙烯基T醯胺和丙烯腈。這些可以單獨使用或聯合使用。 〜當用紫外線輻照固化著色組成物時,將光致聚合引發劑 等添加到本發明的用於濾色器的著色組成物中。 ^致聚合引發劑的例子包括苯乙酮光致聚合引發劑如 4-苯氧基二氯苯乙酮、4-第三丁基一二氯苯乙酮、二乙氧 基苯乙酮、1-(4—異丙基苯基)-2 —羥基—2—甲基丙—丨—酮、 1 -羥基環己基苯甲酮、2一苄基一2 —二甲胺基一丨一以一嗎啉代 苯基)-丁-1-酮和2-甲基-丨一^一(甲硫基)苯基)一2一嗎啉代 丙-1-酮;苯偶姻光致聚合引發劑如苯偶姻、苯偶姻曱醚、 苯偶姻乙醚、苯偶姻異丙醚和苄基二曱基縮酮;二苯曱酮 光致聚合引發劑如二苯曱酮、苯甲醯苯甲酸、曱基苯曱醯 苯亞曱酸酯(methyl benzoylbenzate)、4-苯基二苯曱 酮、羥基二苯曱酮、丙烯酸酯化二苯曱酮和4一笨甲醯基 -4 -曱基二苯硫醚;噻噸酮光致聚合引發劑如噻噸酮、2一 氯噻噸酮、2-曱基噻噸酮、異丙基噻噸酮和2,4—二異丙 基噻噸酮,二啡光致聚合引發劑如2, 4, 三氣—s —三讲、 2-苯基-4, 6-雙(三氯曱基)— s—三讲、2一(對曱氧笨 基)-4, 6-雙-(三氯曱基)— s —三啡、2一(對曱笨基)一4, 6一雙 (二氯曱基)- s-三畊、2-胡椒基—4, 6一雙(三氯曱基)—s 一三 畊、2, 4-雙(二氯曱基)一6 —苯乙烯基一s一三讲、2一(萘醯一工一 基)-4,6-雙(三氯甲基)三啩、2一(4一甲氧基—萘醯一工一 基)-4, 6-雙(三氯甲基)三啡、2,4一三氯曱基一(胡椒 312XP/發明說明書(補件)/95·08/95114255 50 200706604 基)-6-三讲和2, 4-三氯曱基(4, 一甲氧 _三 七喊鹽光致聚合引發劑、㈣光致聚合引發;和㈣ 光致聚合引I劑。在著色組成物中,4 _重量份的顏料 可以使用5到200重量份,較佳1〇到15〇重量份的光致 聚合引發劑。 上述光致聚合引發劑可以被單獨使用或聯合使用。可以 另外使用作為敏化劑的化合物如氧基醋、酿基氧化 •、甲基苯基乙駿酸、节基_9,1〇_菲@昆、获㈣、乙基葱 醌、4’4’-二乙基異二苯代酚酞、3, 3’,4,4,一四(第三丁基 過氧幾基)二苯甲_和4,4,_二乙胺基二苯甲^在著色 組成物中田,每1〇〇重量份的光致聚合引發劑可以使用〇 ι 到6 0重量份的敏化劑。 本發明3的用於濾色器的著色組成物可以以溶劑顯影 類或鹼顯影類著色抗敍劑的形式製備。在該著色抗蝕劑 中,顏料分散在包括熱塑性樹脂、熱固性樹脂或活性能量Cu-pc; copper indigo residue 312XP/invention specification (supplement)/95-〇8/95114255 47 200706604 Then #, the coloring composition for a color filter provided by the present invention will be described, and the coloring composition contains The fine organic pigments and pigments thus obtained. The fine organic pigment is dispersed in a pigment carrier contained in the colored composition of the present invention. The pigment carrier consists of a transparent resin, its precursor or their delta. The transparent resin exhibits a light transmission rate of preferably 80% or more, more preferably 95% or more, over the entire visible wavelength of 4 Å to 7 Å. The transparent resin includes a thermoplastic resin, a thermosetting resin, and an active energy beam curable resin. Its precursors include monomers and oligomers each cured by irradiation with an active energy beam and thereby preparing a transparent resin. These can be used alone or in combination. In the coloring composition, from 3 to 700 parts by weight, preferably from 6 to 450 parts by weight, of the pigment carrier may be used per 100 parts by weight of the pigment. When a mixture of a transparent resin and a precursor thereof is used as a pigment carrier, 20 to 400 parts by weight, more preferably 50 to 250 parts by weight, of the transparent resin per 100 parts by weight of the pigment can be used in the coloring composition. Further, in the coloring composition, from 1 to 300 parts by weight, preferably from 1 to 200 parts by weight, of the precursor of the transparent resin may be used per 100 parts by weight of the pigment. Examples of the thermoplastic resin include butyral resin, styrene-maleic acid copolymer, chlorinated polyethylene, chlorinated polypropylene, polyvinyl chloride, ethylene-vinyl acetate copolymer, polyvinyl acetate, polyurethane resin, Polyester resin, acrylic resin, alkyd resin, polystyrene resin, polyamide resin, rubber resin, cyclized rubber resin, cellulose, polyethylene (HDPE and LDPE), polybutadiene and polyimide resin . Examples of thermosetting resins include Epoxy 312XP/Invention Manual (Supplement)/95-08/95114255 48 200706604 Fat, benzoguanamine resin, rosin-modified maleic acid resin, rosin-modified fumaric acid resin, Polycyanamide resin, urea resin and phenolic resin. • Examples of the active energy beam curable resin include: by reaction between a (fluorenyl)acrylic acid compound having a trans-reactive substituent such as an isocyanate group, an aldehyde group or an epoxy group or cinnamic acid and the above polymer a resin prepared by introducing a photocrosslinking group such as a (meth)acryl fluorenyl group or a styryl group into a polymer having a reactive substituent such as a light group, a group or an amine group, by containing an acid anhydride Preparation of a linear polymer such as a styrene-maleic anhydride copolymer or an α-olefin-maleic anhydride copolymer with a half-esterification of a (meth)acrylic compound having a hydroxyl group such as a hydroxyalkyl (meth) acrylate Resin. Examples of the monomers and oligomers which are precursors of the transparent resin include various acrylates and methacrylates such as (mercapto) decyl acrylate, (mercapto) ethyl acrylate, (mercapto) acrylic acid 2-hydroxyethyl Base ester, 2-hydroxypropyl (mercapto) acrylate, cyclohexyl (meth) acrylate, carboxy-ethyl ruthenium (meth) acrylate, t- allyl (mercapto) acrylate, 1 ,6-hexanediol di(indenyl)acrylate, triethylene glycol di(meth)acrylate, tripropylene glycol di(meth)acrylate, trimethylolpropane tri(meth)acrylate , pentaerythritol tris(meth)acrylate, hydrazine, 6-hexanediol diglycidyl ether di(meth)acrylate, bisphenol A diglycidyl ether di(meth)acrylate, neopenta Alcohol diglycidyl ether di(meth)acrylate, dipentaerythritol hexa(meth)acrylate, tricyclodecenyl (meth)acrylate, ester acrylate, methylol melamine (methyl) Acrylate, epoxy (meth) acrylate and urethane acrylate; Acrylic acid, styrene, acetic acid 312XP / invention manual (supplement) / 95-08/95114255 49 200706604 ethylene s 曰, hydroxyethyl vinyl ether, ethylene glycol divinyl ether, pentaerythritol trivinyl ether, (methyl) propyl Dilute amine, N-methyl (meth) acrylamide, N-vinyl T amide and acrylonitrile. These can be used alone or in combination. When a coloring composition is cured by ultraviolet irradiation, a photopolymerization initiator or the like is added to the coloring composition for a color filter of the present invention. Examples of the polymerization initiator include an acetophenone photopolymerization initiator such as 4-phenoxydichloroacetophenone, 4-tert-butyldichloroacetophenone, diethoxyacetophenone, and 1 -(4-isopropylphenyl)-2-hydroxy-2-methylpropanone-one, 1-hydroxycyclohexyl benzophenone, 2-benzyl-2-dimethylaminol-one-one Morpholinophenyl)-butan-1-one and 2-methyl-indole-methyl(methylthio)phenyl)-dimorpholinopropan-1-one; benzoin photopolymerization initiator Such as benzoin, benzoin oxime ether, benzoin ethyl ether, benzoin isopropyl ether and benzyl dinonyl ketal; benzophenone photopolymerization initiator such as benzophenone, benzamidine Formic acid, methyl benzoylbenzate, 4-phenyl dibenzophenone, hydroxydibenzophenone, acrylated dibenzophenone, and 4-benzoicin-4-yl Diphenyl sulfide; thioxanthone photopolymerization initiators such as thioxanthone, 2-chlorothioxanthone, 2-mercaptothioxanthone, isopropylthioxanthone and 2,4-diisopropylthiophene Tons of ketone, dimorphine photopolymerization initiator such as 2, 4, three gas-s - three lectures, 2-phenyl-4, 6-double ( Chloroguanidinyl) — s—three lectures, two ones (p-oxo-oxyphenyl)-4,6-bis-(trichloroindenyl)-s-tri-morphine, two-one (p-stupyl)-four, 6 A pair of (dichloroindenyl)-s-three-plowing, 2-piperidin- 4,6-double (trichloroindenyl)-s-three-plowing, 2,4-bis(dichloroindenyl)-6 Styryl-s-three-speaking, 2-(naphthoquinone-in-one-based)-4,6-bis(trichloromethyl)triterpene, 2-(4-methoxy-naphthoquinone-in-one-based) -4,6-bis(trichloromethyl)triphthyl, 2,4-trichloroindolyl-(Pepper 312XP/Invention Manual (supplement)/95·08/95114255 50 200706604))-6-three talks 2, 4-trichloroindenyl (4, monomethoxy_37 sulphonic photopolymerization initiator, (iv) photopolymerization initiation; and (iv) photopolymerization initiator. In the coloring composition, 4 _ parts by weight The pigment may be used in an amount of 5 to 200 parts by weight, preferably 1 to 15 parts by weight, based on the photopolymerization initiator. The above photopolymerization initiator may be used singly or in combination. A compound which is a sensitizer may be additionally used. Oxyacetic acid, brewing base oxidation, methyl phenyl benzoic acid, nodal base _9, 1 〇 _ 菲 @昆, obtained , ethyl onion, 4'4'-diethyliso-diphenylphenolate, 3, 3', 4, 4, tetra-(t-butylperoxy)biphenyl- and 4,4, _Diethylaminodibenzoic acid is used in the coloring composition, and a sensitizer may be used in an amount of from 1 to 10 parts by weight per 1 part by weight of the photopolymerization initiator. The color filter of the present invention 3 is used. The colored composition can be prepared in the form of a solvent-developing or alkali-developing coloring anti-synthesis agent. In the colored resist, the pigment is dispersed in a thermoplastic resin, a thermosetting resin or an active energy.

束可固化樹脂和單體的顏料哉_ I 平瓶们顋枓载體中。經由用分散裝置如三 幸昆式研磨機、兩輥式研磨機、以、* 八巧保械砂磨機、揑合機或磨碎機、 將-種或至少兩種微細有機顏料與所需的紐聚合引發 劑-起細細分散到顏料載體中來製備該著色抗韻劑。此 外,通過將至少兩種上述微鈿嚭 ^ , U、,、田顏枓分別分散在顏料載體中 製備刀政體,然後混合該分散體,也可以製備由本發明提 供的用於濾色器的著色組成物。 當顏料分散在顏㈣體中時,根據需要可以使用 劑如樹脂類㈣分散劑、表㈣性劑、料的顏料衍生 312XP/發明說明書(補件)/95-08/95114255 51 200706604 物、蒽醌衍生物”丫咬酮衍生 助劑可以極好地分散顏料廿”并何生物。由於分散 刀政顏科亚且對防止分散後 聚具有很好的效果,t使用通過使用分散將 在顏料載體帽得的著色組成物時,獲得了具有優 ==二色組成物中,㈣重量份的顏料可以 使用0 · 1到4 0重量Y合,於/土 η 1 r*丨η Λ 知較么0· I到30重量份的分散助劑。The bundle of curable resin and monomeric pigment 哉 _ I are in the bottle. By using a dispersing device such as a Sanxun-type grinder, a two-roll mill, an octagonal protective sander, a kneader or an attritor, a seed or at least two kinds of fine organic pigments and a desired New Zealand The polymerization initiator is prepared by finely dispersing into a pigment carrier to prepare the coloring agent. Further, the coloring for the color filter provided by the present invention can also be prepared by dispersing at least two kinds of the above-mentioned micro 钿嚭, U, 、, 枓, 枓, respectively, in a pigment carrier to prepare a knife body, and then mixing the dispersion. Composition. When the pigment is dispersed in the body of the pigment (4), a pigment such as a resin (iv) dispersant, a table (four) agent, and a pigment derivative may be used as needed. 312XP/invention specification (supplement)/95-08/95114255 51 200706604 The hydrazine derivative "bite ketone-derived auxiliaries can disperse the pigment 极 very well" and what organisms. Since dispersing Knife Yankea and having a good effect on preventing post-dispersion polymerization, t is obtained by using a coloring composition which is dispersed in a pigment carrier, and having a composition of excellent == dichroism, (iv) weight The pigment may be used in an amount of from 0. 1 to 40% by weight, and in the range of from 0 to 1 part by weight of the dispersing aid.

〜在适些W助劑中’顏料衍生物、葱⑽生物"丫销 =生物和—啡衍生物(下文中有時—般稱作「衍生物」) 是車乂么的刀政助劑,這是因為這些衍生物對於防止微細有 機顏料的團聚和保持有機顏料被細細分散的狀態具有優 異的功能,並因此通過使用含有至少一種這些衍生物的著 色組成物可以製備具有高對比度和高色純度的滤色器。 樹脂類顏料分散劑具有與顏料有親和力並且可吸附在 顏料上的部分以及與顏料載體相容的部分,它的作用是通 過被吸收在顏料上的方式穩定顏料在顏料載體中的分~ In some W additives, 'pigment derivatives, onion (10) bio " credit sales = biological and - morphine derivatives (hereinafter sometimes referred to as "derivatives") is the knife auxiliaries of the car, This is because these derivatives have an excellent function for preventing agglomeration of fine organic pigments and maintaining a state in which the organic pigments are finely dispersed, and thus can be prepared with high contrast and high color by using a coloring composition containing at least one of these derivatives. Color filter for purity. The resin-based pigment dispersant has a portion having affinity with the pigment and adsorbing on the pigment and a portion compatible with the pigment carrier, and its function is to stabilize the pigment in the pigment carrier by being absorbed on the pigment.

散。遠樹脂類顏料分散劑特別地包括油質分散劑如聚胺 醋、由聚丙烯酸酯代表的聚羧酸酯、不飽和聚醯胺、聚羧 酸、聚羧酸的(部分)胺鹽、聚羧酸的銨鹽、聚羧酸的烷基 胺鹽、聚矽氧烷、長鏈聚胺基醯胺磷酸鹽、含羥基聚羧酸 的醋和它的改性產物、或者通過聚(低級烷撐亞胺)與具有 游離叛基的聚酯反應形成的醯胺、或它的鹽;水溶性樹脂 或水溶性聚合物如(曱基)丙烯酸—苯乙烯共聚物、(曱基) 丙烯酸-(曱基)丙烯酸酯共聚物、苯乙烯—馬來酸共聚物、 聚乙烯醇或聚烯ϋ比酮;聚醋;改性聚丙烯酸環氧乙烧 312ΧΡ/發明說明書(補件)/95-08/95114255 52 200706604 /環氧丙烷和磷酸酯的加合物。這些樹脂類顏料分散劑可 以單獨使用或聯合使用。 表面活性劑包括陰離子表面活性劑如聚氧乙烯烷基醚 硫酸鹽、十二烷基苯磺酸鈉、苯乙烯-丙烯酸共聚物的鹼 金屬鹽、烷基萘磺酸鈉、烷基二笨醚二磺酸鈉、單乙醇胺 月桂基硫酸鹽、三乙胺月桂基硫酸鹽、月桂基硫酸銨、單 乙醇胺硬脂酸鹽、硬脂酸鈉、月桂基硫酸鈉、苯乙烯一丙 烯酸共聚物的單乙醇胺和聚氧乙烯烷基醚磷酸酯;非離子 表面活性劑如聚氧乙烯油烯基醚、聚氧乙烯月桂基醚、聚 氧乙烯壬基苯基醚、聚氧乙烯烷基醚磷酸酯、聚氧乙烯山 梨聚糖一硬脂酸和聚乙二醇一月桂酸;陽離子表面活性劑 如四烷基銨鹽及其環氧乙烷加合物;和兩性表面活性劑如 由烧基二甲胺基醋酸甜菜驗代表的烧基甜菜驗、和燒基味 唑啉。這些表面活性劑可以單獨使用或聯合使用。 為了將顏料充分分散在顏料載體中、並且通過將著色組 成物施加到透明基質如玻璃基質上直至幹膜厚度為〇.2 到5 // m來促進濾色器片的形成,由本發明3提供的用於 濾、色裔的著色組成物可以含有溶劑。 溶劑的例子包括丨,2,3-三氯丙烷、丨,3_丁二醇、丨,3〜 丁一醇、1,3-丁二醇雙醋酸鹽、丨,4_二氧己環、2_庚鲷、 2-f基丙二醇、3 5 5_三甲基_2_環己烯_卜網、 3, 3, 5-三甲基環己_、3_乙氧基丙酸乙酯、3一甲基 丁二醇、3-甲氧基I甲基+丁醇、3一甲氧基_3_甲基乙 酸丁醋、3-甲氧丁醇、甲氧基乙酸丁醋、4_庚酮、間二 312XP/發明說明書(補件)/95-08/95丨14255 53 200706604 曱ί I門乙苯、間二氯苯、N,N—二曱基乙醯胺、N, 一 土甲醯胺、正丁基醇、正丁基苯、乙酸正丙酯、N〜 曱基ϋ比洛烧酉同、鄰-审贫^ „ nl 一甲本、鄰氣曱苯、鄰二乙苯、鄰二秦 苯、對氣甲苯、對-Γ贫结 乳 耵一乙本、苐二丁苯、第三丁苯、 内s曰異丁基醇、異佛爾酮、乙二醇二乙基醚、乙二醇二 丁基醚'乙二醇單異丙基_、乙二醇單乙基醚、乙二醇: 、乙二醇單第三丁基_、乙二醇單丁基醚、乙 二醇皁丁基_乙酸g旨、乙二醇單丙基_、乙二醇單 醚、乙一醇單甲基醚、乙二醇單曱基醚乙酸醋、二異丁酉同、 :伸乙甘醇二乙基醚、二伸乙甘醇二曱基醚、二伸乙甘醇 單異丙基醚、二伸乙甘醇單乙醚乙酸酯、二伸乙甘醇單丁 基喊一伸乙甘醇單丁基醚乙酸酯、二伸乙甘醇單甲基 醚環己醇、環己醇醋酸酯、環己酮、二丙二醇二甲基_、 一丙一醇曱_乙酸酯、二丙二醇單乙基醚、二丙二醇單丁 基醚、二丙二醇單丙基醚、二丙二醇單曱基醚、雙丙酮醇、 一醋精、二丙二醇單丁基醚、三丙二醇單曱基醚、丙二醇 雙醋酸酯、丙二醇苯基醚、丙二醇單乙基醚、丙二醇單乙 輕乙3文|曰丙一醇單丁基_、丙二醇單丙基醚、丙二醇單 曱基鍵、丙二醇單曱基醚乙酸酯、丙二醇單曱基醚丙酸 酯、苄醇、甲基異丁酮、甲基環己醇、乙酸正戊酯、乙酸 正丁醋、乙酸異戊酯、乙酸異丁酯、乙酸丙酯和二元酸酯。 這些洛劑可以單獨使用或聯合使用。在著色組成物中,每 100重量份的顏料可以使用800到4, 000重量份,較佳 1, 0 0 0到2,5 0 0重量份的溶劑。 312ΧΡ/發明說明書(補件)/95·〇8/95丨14255 54 200706604 此外,本發明3提供的用於 有用於隨時間流逝°。的耆色組成物可以含 穩定劑的例黏度的儲存穩定劑。儲存 川于包括弟四銨的氯化物如苄基 !:基錢、有機酸如乳酸和草酸及其甲基驗、第 成ΓΓ如三乙基膦和三苯基膦、和亞磷酸鹽:在 者色組成物中,每彳η η舌旦7八 在Scattered. The far resin-based pigment dispersant specifically includes an oily dispersant such as polyamine vinegar, a polycarboxylate represented by a polyacrylate, an unsaturated polyamine, a polycarboxylic acid, a (partial) amine salt of a polycarboxylic acid, and a poly An ammonium salt of a carboxylic acid, an alkylamine salt of a polycarboxylic acid, a polyoxyalkylene oxide, a long-chain polyamine guanamine phosphate, a hydroxy-containing polycarboxylic acid vinegar and a modified product thereof, or a poly(lower alkane) An indoleamine formed by reacting a polyester having a free rebel group, or a salt thereof; a water-soluble resin or a water-soluble polymer such as a (mercapto)acrylic acid-styrene copolymer, (mercapto)acrylic acid-( Acrylate copolymer, styrene-maleic acid copolymer, polyvinyl alcohol or polyene ketone; polyacetate; modified polyacrylic acid epoxy 312 ΧΡ / invention manual (supplement) / 95-08 /95114255 52 200706604 / Adduct of propylene oxide and phosphate. These resin-based pigment dispersants may be used singly or in combination. Surfactants include anionic surfactants such as polyoxyethylene alkyl ether sulfate, sodium dodecylbenzenesulfonate, alkali metal salts of styrene-acrylic acid copolymers, sodium alkylnaphthalenesulfonate, alkyl diphenyl ethers Single sodium disulfonate, monoethanolamine lauryl sulfate, triethylamine lauryl sulfate, ammonium lauryl sulfate, monoethanolamine stearate, sodium stearate, sodium lauryl sulfate, styrene-acrylic acid copolymer Ethanolamine and polyoxyethylene alkyl ether phosphate; nonionic surfactants such as polyoxyethylene oleyl ether, polyoxyethylene lauryl ether, polyoxyethylene nonylphenyl ether, polyoxyethylene alkyl ether phosphate, Polyoxyethylene sorbitan monostearate and polyethylene glycol monolaurate; cationic surfactants such as tetraalkylammonium salts and ethylene oxide adducts thereof; and amphoteric surfactants such as alkyl methacrylate The amine-based acetic acid beet test represents a burnt beet test, and the burnt-based oxazoline. These surfactants may be used singly or in combination. In order to sufficiently disperse the pigment in the pigment carrier and to promote the formation of the color filter sheet by applying the coloring composition to a transparent substrate such as a glass substrate until the dry film thickness is from 2.2 to 5 // m, provided by the present invention 3 The colored composition for filtration, chromogenic can contain a solvent. Examples of the solvent include hydrazine, 2,3-trichloropropane, hydrazine, 3-butanediol, hydrazine, 3-butanol, 1,3-butanediol diacetate, hydrazine, 4-dioxane, 2_heptanthene, 2-f-propyl propylene glycol, 3 5 5_trimethyl-2-cyclohexene _ net, 3, 3, 5-trimethylcyclohexanyl, ethyl 3-ethoxypropionate , 3-methylbutanediol, 3-methoxylmethyl+butanol, 3-methoxy-3-methylacetate butyl vinegar, 3-methoxybutanol, methoxyacetic acid butyl vinegar, 4 _heptanone, two 312XP/invention manual (supplement)/95-08/95丨14255 53 200706604 曱ί I ethylbenzene, m-dichlorobenzene, N,N-dimercaptoacetamide, N, one Methyl amide, n-butyl alcohol, n-butyl benzene, n-propyl acetate, N~ 曱 ϋ ϋ 洛 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 、 Benzene, o-di-qinylbenzene, p-toluene, p-quinone-poor acetophenone, bis-butylbenzene, tert-butylbenzene, internal s-isobutyl alcohol, isophorone, ethylene glycol Ether, ethylene glycol dibutyl ether 'ethylene glycol monoisopropyl _, ethylene glycol monoethyl ether, ethylene glycol: ethylene glycol mono-tert-butyl _, ethylene glycol monobutyl ether B2 Soap butyl-acetic acid g, ethylene glycol monopropyl _, ethylene glycol monoether, ethyl alcohol monomethyl ether, ethylene glycol monodecyl ether acetic acid vinegar, diisobutyl hydrazine, : ethylene glycol Ethyl ether, diethylene glycol didecyl ether, diethylene glycol monoisopropyl ether, diethylene glycol monoethyl ether acetate, diethylene glycol monobutyl ketone Butyl ether acetate, diethylene glycol monomethyl ether cyclohexanol, cyclohexanol acetate, cyclohexanone, dipropylene glycol dimethyl _, monopropanol oxime acetate, dipropylene glycol single Ethyl ether, dipropylene glycol monobutyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monodecyl ether, diacetone alcohol, monoacetic acid, dipropylene glycol monobutyl ether, tripropylene glycol monodecyl ether, propylene glycol diacetate Ester, propylene glycol phenyl ether, propylene glycol monoethyl ether, propylene glycol, monoethyl phthalate, propylene glycol monobutyl ketone, propylene glycol monopropyl ether, propylene glycol monothiol linkage, propylene glycol monodecyl ether acetate , propylene glycol monodecyl ether propionate, benzyl alcohol, methyl isobutyl ketone, methyl cyclohexanol, n-amyl acetate, n-butyl acetate, isoamyl acetate, acetic acid Butyl ester, propyl acetate and dibasic acid ester. These granules may be used singly or in combination. In the coloring composition, 800 to 4,000 parts by weight, preferably 1,0 0, may be used per 100 parts by weight of the pigment. 0 to 2,500 parts by weight of solvent. 312 ΧΡ / invention specification (supplement) / 95 · 〇 8 / 95 丨 14255 54 200706604 Further, the present invention 3 provides for use in the bleak for use over time. The composition may contain a storage stabilizer of a viscosity of a stabilizer. The storage is carried out in a chloride including tetraammonium such as benzyl!: base money, organic acids such as lactic acid and oxalic acid, and methyl groups thereof, and the like Phosphine and triphenylphosphine, and phosphite: in the color composition, each 彳 η tongue is 7-8

重量份的儲存穩定劑。s刀、可以使用ο.1到U 只要不降―性,本發们提供 組成物可以含有用於調色的染料。…色时的者色 較佳,藉助於例如離^分離器、燒結_檢程式或 :,式從本發明3的著色組成物中去除一或以上: 佳=或以上、更佳U㈣或以上的粗粒子和混合粉塵。 μ後’將說明本發明3的濾色器。 的遽色器包括形成在透明或反射基質表面上 的U R(紅)、G(綠)、Β(藍)、γ(黃)、μ(品紅)或 中至少兩種顏色的濾色器片。根據印刷方法或影印方法, 通過使用本發明提供的用於濾色器的著色組成物可以形 成相應顏色的滤色器片。作為透明基質,可以使 搞 和樹脂板如聚碳酸酉旨、甲基聚甲基丙埽酸醋和聚對苯二 酸乙二醇酯。 τ 在根據印刷方法形成各個濾色器片的過程中,只由重複 印刷和乾燥作為上述各種印刷油墨而進行製備的用於滤 色器的著色組成物就可以形成圖*,因此該印刷方法和製 備濾色器的方法一樣是一種低成本方法而且在大規模生 312ΧΡ/發明說明書(補件)/95-08/95114255 55 200706604 產方面是優秀的。此外,由於印刷技術的發展,可以印刷 具有高尺寸精度和平滑度的精細圖案。對於印刷,油墨不 會乾燥和固化在印刷板或毯子上的情況是較佳的。印刷機 上油墨流動性的控制也是重要的,用分散劑和增量顏料可 以調節油墨的黏度。 當用影印法形成各個濾色器片時,用塗覆方法如喷塗、 旋塗、狹縫塗布或輥塗,將作為溶劑顯影類或鹼顯影類 色抗姓劑製備的著色組成物以〇.2到的乾厚度塗覆 在透明基質上。將根據需要進行乾燥的薄臈通過具有預定 圖案的掩模曝露於紫外線下,上述掩模以與上述薄膜接觸 或不接觸的方式提供。其後,將薄膜浸潰在溶劑或驗性顯 影劑中,或者用喷霧器喷灑顯影劑,除去未顯影的部分以 形成所需的圖案,對於其他顏色重複同樣的程式。這樣, 能夠製備濾色器。為了促進著色抗蝕劑的聚合,根據需要 進行加熱。根據影印法,能夠製備比用印刷方法製備^ 色器精度更高的濾色器。 〜 在顯影中,碳酸鈉或氫氧化鈉水溶液可以用作鹼性顯與 劑、’也可以使用有機鹼如二甲基节胺和三乙醇胺。可以^ 消泡劑或表面活性劑添加到顯影劑中。 為了增加紫外線曝光靈敏度,可以在塗覆和乾燥著 餘劑以後進行紫外線曝光,而且塗覆水溶性紐水溶液可 洛解樹脂、比如聚乙烯醇或水溶性丙烯酸樹脂並且 以形成可防止氧引發的聚合的薄膜。 、 用除上述方法外的電解沉積法或轉移法也能夠製備本 312ΧΡ/發明說明書(補件)/95-08/95114255 ^ 200706604 發明3的濾色器。能夠用任 物。電解沉積法是藉师本發明的著色組成 沉積形成在形成於透日;將各個滤色器片電解 遽色器的方法。此外,轉移=明導電薄膜上以形成 :::基片上’然後將該渡色器層轉移到所需透明基質: (實施例) 在下文中將參考實施例和習知 本發明。然而,本發明並不限制於、:::比較例詳細說明 中,「份」代表「重量份」些實施例。在實施例 (實施例η 伤」心代表「重量%」。 將==—daIr〇nWorks.co.,LTD._, 提供)作H(T—95 粗製藍,由 muhaitoyoinkc〇·,ltd. ^作為有機顏料、600份氣化納作為水溶性無機鹽、 ==乙:::=性有機液體…松香樹脂 emical Industries,Ltd·提 5 ° ,螺计置加料器(圖1中的計量加料器部分4)供給到 w_合機 1〇(「MiracleK. C. K.-型 42」,由 AsadaIr〇n 〇rks. Co.,LTD.提供)中。連續揑合機1()具有直徑 120ηιιηφ的加料部分螺桿和由固定盤和旋轉盤組成的八組 揑合部分。在5〇rpm的主軸轉數和9(TC的揑合溫度下, 、21 kg/】扦的揑合組成物擠出量操作連續揑合機1 〇。用 於揑合的電功率消耗量為每lkg顏料ΐ 8ω。取出由此 312XP/發明說明書(補件)/95_〇8/951 ία% 57 200706604 獲得的被揑合組成物並將其倒入70°C的5, 000份水中。 保持溫度攪拌該混合物1小時,接著過濾,用水洗滌並乾 燥’由此獲得顏料組成物。 將10份上述顏料組成物與90份用於凹印油墨的清漆 (硝酸纖維素樹脂12%、乙酸乙酯33%、曱苯30%、異 丙醇15%和甲醇1〇% )和1〇〇份3-mm玻璃珠混合。用油 漆調節器分散60分鐘以製備凹印油墨。用刮條塗布機# 4 將凹印油墨塗覆在透明薄膜上。將白紙和黑紙放置在由此 獲得的塗覆品的背面上。用比色計分別進行比色。亮度 L*的差數(^L*)為5.2。Δί*通常用作透明度的標準。當 △ L*較大時,透明度越好。 下面說明比較例1和2,其中用常用的容量為i〇〇〇體 積份的雙臂揑合機進行揑合。比較例丨不含作為普通揑合 材料成分的樹脂。雖然實施例1中電功率的消耗量小於比 車父例1中電功率的消耗量,但是實施例i的凹印油墨塗覆 品在透明度上要優於比較例丨的凹印油墨塗覆品。比較例 2與貫施例1的使用成分相同,也包括樹脂。比較例2的 凹印油墨塗覆ππ在透明度上要優於比較例1的凹印油墨 塗覆品。由此發現添加樹脂的效果。然而,實施例丨中的 透明度要優於比較例2。作為揑合裝置,連續揑合機要優 於雙臂揑合機。 下面說明比較例3和4,其中揑合材料不含樹脂而且使 用實施例1中使用的連續揑合機。雖然比較例3的揑合條 件與實施例1的相同,但是比較例3中的凹印油墨塗覆品 312XP/發明說明書(補件)/95-08/95114255 58 200706604 的透明度較差。因此,可以認識到實施例丨中添加樹脂的 ,果。比較例4降低了比較例3所用的水溶性有機液體的 量並且通過加倍電功率消耗量增加了揑合能量。比較例4 中的凹印油墨塗覆品的透明度與比較例3的大致相同。當 揑合材料不含樹脂時,在改進凹印油墨塗覆品的透明度上 是受限的。 基於上述結果,由於使用連續揑合機以及在揑合材料中 混入樹脂可以用少量的能量獲得具有良好的由透明度代 表的實際質量的顏料組成物。 (比較例1) 將 100 份藍 15CT-95 粗製藍,由 ZHUHAI T〇Y〇 INK c〇., LTD·提供)作為有機顏料、6〇〇份氯化鈉作為水溶性無機 鹽和100份二伸乙甘醇作為水溶性有機液體置於容量為 1 000體積份的雙臂揑合機中。在9〇。。揑合該混合物5小 時同,該f合物保持在稠密漿體狀態。揑合所需的電功率 消耗罝為每lkg顏料4. lkwh。取出由此獲得的被揑合也 成物並將其倒人⑽的5,刚份水中。料溫度授掉該 混合物1小時,接著過濾,用水絲並乾燥,由此獲得顏 料組成物。以與實施例1 g A . 貝她例1同樣的方式使用上述顏料組成物 獲得塗覆品。塗覆品的△ [*為丨.2。 (比較例2 ) 將 100 份藍 15(τ—95 粗製藍,由 ZHUHAITOYOINKCO. LTD.提供)作為有機顏料、_錢仙作為水溶性無機 鹽、100伤—伸乙甘醇作為水溶性有機液體和5份松香樹 312XP/發明說明書(補件)/95-08/95114255 59 200706604 月曰(酉曰树膠 AT’ 由 Arakawa Chemical Industries,Ltd·Parts by weight of storage stabilizer. s knife, you can use ο.1 to U as long as it does not drop the sex, the hair supply of the composition can contain the dye used for toning. Preferably, the color of the color is preferably one or more removed from the coloring composition of the present invention by means of, for example, a separator, a sintering method, or a formula: preferably = or more, more preferably U (four) or more. Coarse particles and mixed dust. The color filter of the present invention 3 will be described after μ. The color filter includes color filter sheets of UR (red), G (green), krypton (blue), gamma (yellow), μ (magenta) or at least two colors formed on the surface of the transparent or reflective substrate. . According to the printing method or the photolithography method, the color filter sheets of the respective colors can be formed by using the coloring composition for a color filter provided by the present invention. As a transparent substrate, it is possible to use a resin plate such as polycarbonate, methyl polymethyl acrylate, and polyethylene terephthalate. τ In the process of forming the respective color filter sheets according to the printing method, the coloring composition for the color filter prepared by repeating printing and drying as the above various printing inks can form a pattern*, and thus the printing method and The method of preparing the color filter is also a low-cost method and is excellent in the production of a large-scale 312 ΧΡ / invention specification (supplement) / 95-08/95114255 55 200706604. In addition, due to the development of printing technology, fine patterns with high dimensional accuracy and smoothness can be printed. For printing, it is preferred that the ink does not dry and solidify on a printing plate or blanket. Control of ink flow on the press is also important, and the viscosity of the ink can be adjusted with dispersants and extender pigments. When each of the color filter sheets is formed by photolithography, a coloring composition prepared as a solvent developing or alkali developing color-resistant anti-surname agent is coated by a coating method such as spraying, spin coating, slit coating or roll coating. The dry thickness of .2 is applied to a transparent substrate. The thin enamel which is dried as needed is exposed to ultraviolet rays through a mask having a predetermined pattern which is provided in contact with or not in contact with the above film. Thereafter, the film is dipped in a solvent or an illustrative developer, or the developer is sprayed with a sprayer to remove the undeveloped portion to form a desired pattern, and the same procedure is repeated for other colors. In this way, a color filter can be prepared. In order to promote the polymerization of the colored resist, heating is carried out as needed. According to the photolithography method, it is possible to prepare a color filter which is more precise than a coloring method by a printing method. ~ In development, an aqueous solution of sodium carbonate or sodium hydroxide can be used as an alkaline sensitizer, and an organic base such as dimethyl ketamine and triethanolamine can also be used. An antifoaming agent or a surfactant may be added to the developer. In order to increase the sensitivity of ultraviolet exposure, ultraviolet exposure may be performed after coating and drying the residual agent, and coating a water-soluble aqueous solution may dissolve a resin such as polyvinyl alcohol or a water-soluble acrylic resin to form an oxygen-inhibited polymerization. film. The color filter of the invention No. 3 312 / invention specification (supplement) / 95-08/95114255 ^ 200706604 can also be prepared by an electrolytic deposition method or a transfer method other than the above method. Can use anything. The electrolytic deposition method is a method in which the coloring composition of the present invention is deposited and formed in a transparent day; a color filter is electrolyzed for each color filter sheet. Further, the transfer = on the conductive film to form a ::: substrate" and then transfer the color filter layer to the desired transparent substrate: (Embodiment) Hereinafter, the present invention will be described with reference to the embodiments and the present invention. However, the present invention is not limited to the following: ":" In the detailed description of the comparative example, "parts" means "parts by weight". In the embodiment (example η injury) the heart represents "% by weight". ==-daIr〇nWorks.co.,LTD._, provided) as H (T-95 crude blue, by muhaitoyoinkc〇·,ltd. ^ As an organic pigment, 600 parts of gasified sodium as a water-soluble inorganic salt, == B:::= organic liquid... rosin resin emical Industries, Ltd. 5 °, screw meter feeder (metering feeder in Figure 1 Part 4) is supplied to the w_he machine 1 ("Miracle K. CK-type 42", supplied by Asada Ir〇n 〇rks. Co., LTD.). The continuous kneading machine 1 () has a feeding portion screw having a diameter of 120 η ιηφ And eight sets of kneading parts composed of a fixed disk and a rotating disk. The kneading composition of the spindle rotation number at 5 rpm and the kneading temperature of 9 (TC kneading temperature, 21 kg / 扦) is operated by the continuous kneading machine 1 〇 The electric power consumption for kneading is 8ω per lkg of pigment 。. The kneaded composition obtained by this 312XP/invention specification (supplement)/95_〇8/951 ία% 57 200706604 is taken out and poured into 70°. 5,000 parts of water in C. The mixture was stirred for 1 hour while maintaining the temperature, followed by filtration, washing with water and drying. 10 parts of the above pigment composition and 90 parts of varnish for gravure ink (nitrocellulose resin 12%, ethyl acetate 33%, toluene 30%, isopropanol 15% and methanol 1%) Mix with 1 part of 3-mm glass beads. Disperse with a paint adjuster for 60 minutes to prepare a gravure ink. Apply a gravure ink to the transparent film with a bar coater #4. Place the white and black paper. On the back side of the thus obtained coated article, the colorimetric was separately performed with a colorimeter. The difference in luminance L* (^L*) was 5.2. Δί* is generally used as a standard for transparency. When ΔL* is large The transparency was better. The following Comparative Examples 1 and 2 were carried out in which a kneading was carried out using a conventional two-arm kneader having a capacity of i〇〇〇. The comparative example contained no resin as a component of a conventional kneading material. The consumption of the medium electric power is less than the consumption of the electric power in the first example, but the gravure ink coating of the embodiment i is superior in transparency to the gravure ink coating of the comparative example. Comparative Example 2 and The composition used in Example 1 was the same, and also included the resin. The gravure ink of Comparative Example 2 was coated with π. π is superior in transparency to the gravure ink coating of Comparative Example 1. Thus, the effect of adding a resin was found. However, the transparency in the Example 要 was superior to that of Comparative Example 2. As a kneading device, the continuous kneading machine was excellent. The two-arm kneader is described below. Comparative Examples 3 and 4 are described below, in which the kneaded material contains no resin and the continuous kneader used in Example 1 is used. Although the kneading conditions of Comparative Example 3 are the same as those of Example 1, Comparative Example 3 The gravure ink-coated article 312XP/invention specification (supplement)/95-08/95114255 58 200706604 has poor transparency. Therefore, it can be appreciated that the resin is added to the examples. Comparative Example 4 reduced the amount of the water-soluble organic liquid used in Comparative Example 3 and increased the kneading energy by doubling the electric power consumption. The transparency of the gravure ink-coated article in Comparative Example 4 was substantially the same as that of Comparative Example 3. When the kneaded material contains no resin, it is limited in improving the transparency of the gravure ink coated article. Based on the above results, since a continuous kneader is used and a resin is mixed in the kneaded material, a pigment composition having a good actual quality represented by transparency can be obtained with a small amount of energy. (Comparative Example 1) 100 parts of blue 15CT-95 crude blue, supplied by ZHUHAI T〇Y〇INK c〇., LTD.) as an organic pigment, 6 parts of sodium chloride as a water-soluble inorganic salt and 100 parts of two Ethylene glycol was placed as a water-soluble organic liquid in a two-arm kneader having a capacity of 1 000 parts by volume. At 9 〇. . The mixture was kneaded for 5 hours, and the compound was kept in a dense slurry state. The electric power required for kneading is 4 0.4 lkwh per lkg of pigment. The thus obtained kneaded product was taken out and poured into the fresh water of 5 (10). The mixture was allowed to pass for 1 hour, then filtered, and the mixture was dried with water, whereby a pigment composition was obtained. The coated product was obtained in the same manner as in Example 1 g A. The △ [* is 丨.2 of the coated product. (Comparative Example 2) 100 parts of Blue 15 (τ-95 crude blue, supplied by ZHUHAITOYOINKCO. LTD.) as an organic pigment, _ Qianxian as a water-soluble inorganic salt, 100-gly-ethylene glycol as a water-soluble organic liquid and 5 parts rosin tree 312XP / invention manual (supplement) / 95-08/95114255 59 200706604 曰 曰 (eucalyptus gum AT' by Arakawa Chemical Industries, Ltd.

提供)置於容量為1 000體積份的雙臂揑合機中。在90°C 揑合該混合物5小時同時該混合物保持在稠密漿體狀 態。捏合所需的電功率消耗量為每lkg顏料4· lkwh。取 出由此獲得的被揑合組成物並將其倒入7(TC的5, 000份 X中保持/JDL度攪拌該混合物1小時,接著過濾,用水洗 滌並乾燥,由此獲得顏料組成物。以與實施例丨同樣的方 式使用上述顏料組成物獲得塗覆品。塗覆品的為 2· 3。 (比較例3)Provided) placed in a two-arm kneader having a capacity of 1 000 parts by volume. The mixture was kneaded at 90 ° C for 5 hours while the mixture was maintained in a dense slurry state. The electric power consumption required for kneading is 4 lkwh per lkg of pigment. The kneaded composition thus obtained was taken out and poured into 7 (500 parts of TC, held in 5,000 parts of X/JDL degree, and the mixture was stirred for 1 hour, followed by filtration, washing with water and drying, thereby obtaining a pigment composition. The coated article was obtained in the same manner as in Example 使用 using the above pigment composition. The coated article was 2.3. (Comparative Example 3)

用轉換混合器(由Asada Iron Works.Co·,LTD·提供), ,100 份藍 15(T-95 粗製藍,由 ZHUHAI τ〇γ〇 INKC〇 ·,LTD 提供)、作為有機顏料、6〇〇份氯化鈉作為水溶性無機鹽和 10〇a伤一伸乙甘醇作為水溶性有機液體近乎均勻地預混5 刀釦以與κ施例1同樣的方式用連續揑合機丨〇揑合並 ,理j此a物以獲得顏料組成物。揑合所需的電功率消耗 量為每lkg顏料L8kwh。其塗覆品的為3 6。 (比較例4) 用轉換,合器(由 Asada Irc)nWQrks· CQ·,LTD•提供), f 100 份藍 15(T—95 粗製藍,由 ZHUHAITOYOINKCO·,LTD· 提t、)作為有;顏料、_❾氯化納作為水溶性無機鹽和 80伤一伸乙甘酉予作為水溶性有機液體近乎均句& 5 分鐘:以與實施例1同樣的方式用連續揑合機10揑合並 处里U亥此口物以獲知顏料組成物。揑合組成物的擠出量為 3 ΠΧΡ/發明說明書(補件矽孓⑽95丨14255 200706604 18kg/小時。揑合所需的電功率消耗量為每丨“顏料 3· 6kwh。其塗覆品的△ L*為3. 7。 ·(實施例2到4) 除了分別用合成松香(Dymerex樹脂,由RikaHercules 提供)、歧化松香(Rondis R,由 Arakawa Chemical Industries,Ltd·提供)和氫化松香(Staybelite 樹脂, 由Rika Hercules提供)代替樹脂外,以與實施例1同樣 的方式獲得顏料組成物。表1顯示了揑合所需的電功率消 耗量和塗覆品的△ L*值。 母個塗覆品的△ L*都大於比較例1到4的值,而且每 個塗覆品都具有良好的透明度。 (實施例5到7和比較例5到7) 在表1所示的揑合條件下分別揑合具有表1所示成分的 揑合材料。以與實施例1同樣的方式分別處理這些材料以 獲得顏料組成物。實施例5和比較例5中所用的有機顏料Using a conversion mixer (supplied by Asada Iron Works. Co., LTD.), 100 parts of Blue 15 (T-95 crude blue, supplied by ZHUHAI τ〇γ〇INKC〇·, LTD), as an organic pigment, 6〇 The sodium chloride was kneaded as a water-soluble inorganic salt and 10 〇a-de-ethylene glycol as a water-soluble organic liquid, and uniformly kneaded in a continuous kneader in the same manner as in the κ application example. This material is obtained to obtain a pigment composition. The electric power consumption required for kneading is L8kwh per lkg of pigment. Its coated product is 36. (Comparative Example 4) Using conversion, a combiner (provided by Asada Irc) nWQrks·CQ·, LTD•), f 100 parts of blue 15 (T-95 crude blue, by ZHUHAITOYOINKCO·, LTD· mention t,) as; Pigment, ❾ ❾ ❾ ❾ 作为 作为 作为 作为 作为 作为 作为 作为 作为 ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ ❾ The mouthpiece is used to know the pigment composition. The kneading composition was extruded in an amount of 3 ΠΧΡ / invention specification (supplement 矽孓 (10) 95 丨 14255 200706604 18 kg / hr. The electric power consumption required for kneading was 3·6 kwh per 。 pigment. Δ L* of the coated product 3.7 (Examples 2 to 4) In addition to synthetic rosin (Dymerex resin, supplied by Rika Hercules), disproportionated rosin (Rondis R, supplied by Arakawa Chemical Industries, Ltd.), and hydrogenated rosin (Staybelite resin), respectively Rika Hercules provided) in place of the resin, the pigment composition was obtained in the same manner as in Example 1. Table 1 shows the electric power consumption required for kneading and the ΔL* value of the coated article. * are larger than the values of Comparative Examples 1 to 4, and each of the coated articles has good transparency. (Examples 5 to 7 and Comparative Examples 5 to 7) Kneaded separately under the kneading conditions shown in Table 1 Kneaded materials of the components shown. These materials were separately treated in the same manner as in Example 1 to obtain a pigment composition. The organic pigments used in Example 5 and Comparative Example 5

⑩為 C· I·顏料黃 i38(Paliotol Yellow K0691HD,由 BASF 提供),實施例6和比較例6中所用的有機顏料為c·丨·顏 料紅 177(Chromophthal Red A2B,由 Ciba Specialty10 is C·I·Pigment Yellow i38 (Paliotol Yellow K0691HD, supplied by BASF), and the organic pigment used in Example 6 and Comparative Example 6 is c·丨·颜红红 177 (Chromophthal Red A2B, by Ciba Specialty

Chemicals Co·提供),實施例7和比較例7中所用的有機 顏料為 C· I·顏料紫 23(Sumiton Fast Violet RL Base, - 由 Sumitomo Chemical Co·,Ltd·提供)。 在實施例5到7中,由用少量電功率消耗量獲得的顏料 組成物製備的塗覆品的△ L*值大於比較例5到7中的值, 而且實施例5到7中的透明度是很好的。 312XP/發明說明書(補件)/95_08/95丨14255 61 200706604 表1The organic pigment used in Example 7 and Comparative Example 7 was C.I. Pigment Violet 23 (supplied by Sumitomo Chemical Co., Ltd.). In Examples 5 to 7, the ΔL* value of the coated article prepared from the pigment composition obtained with a small amount of electric power consumption was larger than that in Comparative Examples 5 to 7, and the transparency in Examples 5 to 7 was very high. Ok. 312XP/Invention Manual (supplement)/95_08/95丨14255 61 200706604 Table 1

揑合機名稱 揑合溫度°C 擠出量或捏合時間 電功率消耗量 kwh/kg Ex. 1 連續揑合機 90 21kg/小時 1.8 CEx. 1 雙臂揑合機 90 5小時 4. 1 CEx. 2 雙臂揑合機 90 5小時 4. 1 CEx. 3 連續揑合機 90 21kg/小時 1. 8 CEx. 4 連續揑合機 90 18kg/小時 3. 6 Ex. 2 連續揑合機 90 21kg/小時 1.8 Ex. 3 連續揑合機 90 21kg/小時 1.8 Ex. 4 連續揑合機 90 21kg/小時 1. 8 Ex. 5 連續揑合機 80 21kg/小時 1.6 CEx. 5 雙臂揑合機 80 5小時 3. 4 Ex. 6 連續揑合機 100 21kg/小時 2. 2 CEx. 6 雙臂揑合機 100 5小時 4. 2 Ex. 7 連續揑合機 80 21kg/小時 2. 3 CEx. 7 雙臂揑合機 80 5小時 4. 7 Εχ·=實施例,CEx.=比較例 312XP/發明說明書(補件)/95-08/95114255 62 200706604 表1 (續)Kneading machine name kneading temperature °C Extrusion amount or kneading time Electric power consumption kwh/kg Ex. 1 Continuous kneading machine 90 21kg/hour 1.8 CEx. 1 Two-arm kneading machine 90 5 hours 4. 1 CEx. 2 Two-arm kneading machine 90 5 hours 4. 1 CEx. 3 Continuous kneading machine 90 21kg / hour 1. 8 CEx. 4 Continuous kneading machine 90 18kg / hour 3. 6 Ex. 2 Continuous kneading machine 90 21kg / hour 1.8 Ex. 3 Continuous kneading machine 90 21kg/hour 1.8 Ex. 4 Continuous kneading machine 90 21kg/hour 1. 8 Ex. 5 Continuous kneading machine 80 21kg/hour 1.6 CEx. 5 Double-arm kneading machine 80 5 hours 3. 4 Ex. 6 Continuous kneading machine 100 21kg/ 2 CEx. 6 Two-arm kneading machine 100 5 hours 4. 2 Ex. 7 Continuous kneading machine 80 21kg/hour 2. 3 CEx. 7 Two-arm kneading machine 80 5 hours 4. 7 Εχ·=Example, CEx .=Comparative example 312XP/Invention manual (supplement)/95-08/95114255 62 200706604 Table 1 (continued)

Εχ·=實施例,CEx, (實施例8) 用轉換混合器(由Asada Iron Works· Co·,LTD提供),Εχ·=Example, CEx, (Example 8) Using a conversion mixer (supplied by Asada Iron Works Co., LTD),

將 100 份藍 15(T-95 粗製藍,由 ZHUHAI Τ0Υ0 INKCO· LTD 提供)作為有機顏料、600份氯化鈉作為水溶性盔機鴎、 100份二伸乙甘醇作為水溶性有機液體和5份前^的二合 物(1)作為衍生物近乎均勻地預混5分鐘。將得到的混ς 物通過螺桿式計量加料器(圖i中的計量加料器部分2 給到連續揑合機1 〇(「Miracle K· C· K -创49山 八 τ w 1 ^ i 42」’由 Asa(ja100 parts of Blue 15 (T-95 crude blue, supplied by ZHUHAI Τ0Υ0 INKCO· LTD) as organic pigment, 600 parts of sodium chloride as water-soluble helmet, 100 parts of diethylene glycol as water-soluble organic liquid and 5 The prepolymer (1) was pre-mixed as a derivative almost uniformly for 5 minutes. The obtained mixed product was fed to a continuous kneader 1 by a screw type metering feeder (the metering feeder portion 2 in Fig. i ("Miracle K·C·K - 创49山八瓦 w 1 ^ i 42"' By Asa(ja

Iron^ks. C。·,LTD.提供)中。連續揑合機i() 徑12〇mfflp的加料部分螺桿和由固定盤和旋轉盤龟 八組揑合部分。在5Qrpm的絲轉數和⑽。C的揑入、田产 下’以21kg/小時的揑合組成物擠出量操 :: .揑合所需的電功率消耗量騎lkg顏料17kw;1 312XP/發明說明書(補件)/95·〇8/95114255 63 200706604 出由此K于的被揑合組成物並將其倒入^的&刚份 水中。保持溫度授拌該混合物1小時,接著過濾,用水洗 A並乾&此獲得顏料組成物。根據順方法,該顏料 組成物具有9〇m2/g的比表面積。將】〇份上述顏料組成物 ” 90伤用於凹印油墨的清漆(硝酸纖維素樹脂μ%、乙 酸乙酯33%、甲苯3〇%、異丙醇⑽和甲醇)和1〇〇 伤3 mm玻祸珠此合。用油漆調節器分散⑽分鐘以製備凹 印油墨。用刮條塗布機#4將凹印油墨塗覆在透明薄膜 上。測量由此獲得的塗覆品的6〇。_光澤度值。該光澤度 值為82%。 下面說明比較例8和9’其中用常用的容量為1〇〇〇體 積份的雙臂揑合機進行揑合。比較例8不含作為普通捏合 材料成分的衍生物。雖然實_ 8中電功率的消耗量小於 比較例8中電功率的消耗量’但是實施例8的顏料組成物 的比表面積大於比較例8而且實施例8的顏料組成物被粉 碎得更細。實施例8的凹印油墨塗覆品的光澤度值較高並 因此具有良好的實際質量。比較例9與實施例8中使用的 成分相同,也包括衍生物。與比較例8相比,比較例9的 顏料組成物的比表面積更大,其凹印油墨塗覆品的光澤度 值更高。因此,可以發現添加衍生物的效果。然而,實施Iron^ks. C. ·, LTD. provided). The continuous kneading machine i() has a feeding portion of a screw of 12 〇mfflp and a kneading portion of eight sets of a fixed disk and a rotating disk turtle. The number of filament revolutions at 5Qrpm and (10). C pinching, field yielding 'Extrusion amount of 21kg/hour kneading composition:: . Electric power consumption required for kneading riding lkg pigment 17kw; 1 312XP / invention manual (supplement) / 95 · 〇 8 / 95114255 63 200706604 The kneaded composition thus obtained is poured into the & The mixture was stirred for 1 hour while maintaining the temperature, followed by filtration, washing with water A and drying & this to obtain a pigment composition. According to the cis method, the pigment composition has a specific surface area of 9 〇 m 2 /g. 90 parts of the above pigment composition" varnish for gravure ink (nitrocellulose resin μ%, ethyl acetate 33%, toluene 3 %, isopropyl alcohol (10) and methanol) and 1 〇〇 3 The mm-glass beads were mixed. The gravure ink was prepared by dispersing for 10 minutes with a paint conditioner. The gravure ink was coated on the transparent film with a bar coater #4. The thus obtained coated article was measured 6 inches. _ Gloss value: The gloss value is 82%. The following Comparative Examples 8 and 9' are described in which a kneading is carried out using a two-arm kneader having a usual capacity of 1 part by volume. Comparative Example 8 does not contain as an ordinary kneading material. A derivative of the component. Although the amount of electric power consumed in the actual battery is smaller than the amount of electric power consumed in Comparative Example 8, the specific surface area of the pigment composition of Example 8 was larger than that of Comparative Example 8 and the pigment composition of Example 8 was pulverized. The gravure ink coated article of Example 8 has a higher gloss value and thus has a good actual quality. Comparative Example 9 is the same as the component used in Example 8, and also includes a derivative. Specific surface area of the pigment composition of Comparative Example 9 Larger, the gravure ink coating has a higher gloss value. Therefore, the effect of adding a derivative can be found. However, implementation

例8中的效果要優於比較例9中的效果。作為揑合裝置, 連續揑合機要優於雙臂揑合機。 σ X 下面說明比較例1G和1卜其中揑合材料*含衍生物而 且使用實施例8中使用的連續揑合機。雖然比較例1〇的 312χΡ/發明說明書(補件)/95-08/95114255 64 200706604 揑合條件與實施例8的i日ΓΠ > ^ 相间,但是比較例10的顏料組成 、,。、口 /貝較小而且其凹印油墨塗覆品的光澤度較 ,夂可以⑽°戠到貫施例8中添加衍生物的效*。比較例 幾=㈣、、1G _所肖的水溶性錢㈣的量並通過 、σ ’、功率 >肖耗1增加了揑合能量。比較例η中, 顏料組成物的比表面積和凹印油墨塗覆品的光澤度值與 又例ig巾的Α致相同。#揑合材料的成分不含衍生物 時,在細碎進度和實際質量上是受限的。 由以上結果可以發現’由於使用了連續揑合機並且在捏 二材料中加入了本發明的衍生物,可以利用少量的能量進 行顏料的細碎,並且改進了實際質量。 (比較例8) 將 100 伤監 15(τ-95 粗製藍,由 ZHUHAI T〇Y〇 INK c〇., ltd.提供)作為有機顏料、6〇〇份氣化鈉作為水溶性無機 孤和100伤一伸乙甘醇作為水溶性有機液體置於容量為 ?〇〇體積份的雙臂揑合機中。在1〇rc揑合該混合物5: 時同$該混合物保持在稠密漿體狀態。揑合所需的電功率 消耗量為每lkg顏料4. Okwh。取出由此獲得的被捏合組 成物並將其倒入70。⑽5, 〇〇〇份水中。保持溫度擾拌該 混合物1小時,接著過濾,用水洗滌並乾燥,由此獲得顏 料組成物。根據BET方法,該顏料組成物具有69mVg的 比表面積。以與實施例8同樣的方式獲得塗覆品。該塗覆 品的光澤度值為66%。 (比較例9) 312XP/發明說明書(補件)/95-08/95114255 65 200706604 將⑽份藍⑼τ,粗製藍,&施 =,LTi).提供)作為有機顏料、_ w作為水溶性 ‘、、、機鹽、m份二伸乙甘醇作為水溶性有機液體和5份前 :的化合物⑴作為衍生物置於容量4 1〇〇〇體積份的雙 機中。㈣rc揑合該混合物5小時同時該混合物 保持在稠錢體狀態。揑合所需的電功率消耗量為每~ 顏料4.1kwh。取出由此獲得的被揑合組成物並將其倒入 :〇C的5’000份水中。保持溫度攪拌該混合物工小時,接 著過濾,用水洗滌並乾燥’由此獲得顏料組成物。根據 BET方法,該顏料組成物具有77m7g的比表面積。以盥實 施例8同樣的方式獲得塗覆品。該塗覆品的 值為 72%。 (比較例10) 用轉換混合器(由Asada Iron Works.Co·,LTD·提供),The effect in Example 8 was superior to that in Comparative Example 9. As the kneading device, the continuous kneading machine is superior to the two-arm kneading machine. σ X Next, Comparative Examples 1G and 1 in which the kneading material* contains a derivative and the continuous kneader used in Example 8 were used. Although the kneading conditions of the 312 χΡ/invention specification (supplement)/95-08/95114255 64 200706604 of Comparative Example 1 were the same as those of Example 8, the pigment composition of Comparative Example 10 was obtained. The mouth/shell is smaller and the gloss of the gravure ink coating is higher, and the effect of adding the derivative in the example 8 can be obtained by (10) °. In the comparative example, the amount of water-soluble money (4), which is (1), and 1G, is increased by kneading energy by σ ′, power > In Comparative Example η, the specific surface area of the pigment composition and the gloss value of the gravure ink coated article were the same as those of the ig towel. # The composition of the kneaded material is not limited, and is limited in the fineness and actual quality. From the above results, it was found that since the continuous kneader was used and the derivative of the present invention was added to the kneaded material, fine powder of the pigment was used with a small amount of energy, and the actual quality was improved. (Comparative Example 8) 100 Injury 15 (τ-95 crude blue, supplied by ZHUHAI T〇Y〇INK c〇., ltd.) as an organic pigment, 6 parts of sodium carbonate as a water-soluble inorganic orphan and 100 The acetaminophen was placed as a water-soluble organic liquid in a two-arm kneader having a volume of 〇〇. When the mixture 5 was kneaded at 1 〇rc, the mixture was kept in a dense slurry state. The electric power required for kneading is 4. Okwh per lkg of pigment. The kneaded composition thus obtained was taken out and poured into 70. (10) 5, 〇〇〇 water. The mixture was stirred at a temperature for 1 hour, followed by filtration, washing with water and drying, whereby a pigment composition was obtained. According to the BET method, the pigment composition had a specific surface area of 69 mVg. A coated article was obtained in the same manner as in Example 8. The coating had a gloss value of 66%. (Comparative Example 9) 312XP/Invention Manual (Supplement)/95-08/95114255 65 200706604 (10) parts of blue (9) τ, crude blue, & s, LTi). Provided as an organic pigment, _ w as a water-soluble ' And, a machine salt, m part of diethylene glycol as a water-soluble organic liquid, and 5 parts of the former compound (1) were placed as a derivative in a double unit having a volume of 41 parts by volume. (d) rc was kneaded for 5 hours while the mixture was kept in a state of thick money. The electric power consumption required for kneading is 4.1 kwh per ~ pigment. The kneaded composition thus obtained was taken out and poured into 5'000 parts of water of 〇C. The mixture was stirred while maintaining the temperature, followed by filtration, washing with water and drying. Thus, a pigment composition was obtained. According to the BET method, the pigment composition had a specific surface area of 77 m7g. The coated article was obtained in the same manner as in Example 8. The coated product had a value of 72%. (Comparative Example 10) Using a conversion mixer (provided by Asada Iron Works. Co., LTD.),

將 100 份藍 15(T-95 粗製藍,由 ZHUHAI TOYO INKCO·,LTD 提供)作為有機顏料、600份氯化鈉作為水溶性無機鹽和 100份二伸乙甘醇作為水溶性有機液體近乎均勻地預混5 分鐘。以與實施例8同樣的方式用連續揑合機1〇揑合和 處理該混合物以獲得顏料組成物。揑合所需的電功率消耗 量為每hg顏料1· 7kwh。根據BET方法,該顏料組成物 具有81m2/g的比表面積。其塗覆品的光澤度值為75%。 (比較例11) 用轉換混合為(由Asada Iron Works· Co·,LTD·提供), 將 100 份藍 15(T-95 粗製藍,由 ZHUHAI TOYO iNK c〇· 312XP/發明說明書(補件)/95-08/95114255 66 200706604 LTD.提供)作為有機顏料、600 p氣彳& 鹽和80份二伸乙例化㈣為水溶性無機 混δ分鐘。以盥眚紘如0 、 ·^丁 1 9地預 人和處理$、、B二“ 同樣的方式用連續揑合機1〇揑 勿以獲得顏料組成物。揑合組成物擠出量 ‘、、、g 4。揑合所需的電功率消耗量為每lkg $_ 3.5kwh。根據BET方、本—* , 甘ug顏枓 矣而择^ 顏料組成物具有82m2々的比 乂知。八'主覆品的光澤度值為76%。 (實施例9到11)100 parts of Blue 15 (T-95 crude blue, supplied by ZHUHAI TOYO INKCO·, LTD) as organic pigment, 600 parts of sodium chloride as water-soluble inorganic salt and 100 parts of diethylene glycol as a water-soluble organic liquid nearly uniform Premix for 5 minutes. This mixture was kneaded and treated with a continuous kneader 1 in the same manner as in Example 8 to obtain a pigment composition. The electric power consumption required for kneading is 1·7 kwh per hg of pigment. According to the BET method, the pigment composition had a specific surface area of 81 m 2 /g. The coated article had a gloss value of 75%. (Comparative Example 11) Using conversion mixing (provided by Asada Iron Works Co., LTD.), 100 parts of blue 15 (T-95 crude blue, by ZHUHAI TOYO iNK c〇· 312XP/invention specification (supplement) /95-08/95114255 66 200706604 LTD. Provided as an organic pigment, 600 p gas 彳 & salt and 80 parts of bismuth (formula) is a water-soluble inorganic mixed δ min. For example, the amount of the composition of the kneading composition is not obtained by the continuous kneading machine 1 in the same manner as the treatment of $, and B. g 4. The electric power consumption required for kneading is $_3.5kwh per lkg. According to the BET side, the present-*, the ug ug, and the pigment composition has a ratio of 82m2 。. The gloss value is 76%. (Examples 9 to 11)

除了分別用化合物⑵、化合物(3)和化合物⑷代替實 施例8中所用的衍生物外,以與實施例8同樣的方式獲得 顏料組成物。纟2顯示了揑合所f的電功率消耗量、根據 BET方法的比表面積和塗覆品的光澤度值。 實施例9到11中的顏料組成物的BET法比表面積和塗 覆品的光澤度值大於比較例8到11中的值。 (實施例12到14和比較例12到14) 在表2所示的揑合條件下分別揑合具有表2所示成分的 揑合材料。以與實施例8同樣的方式分別處理這些材料以 獲得顏料組成物。實施例12和比較例12中使用的有機顏 料為 C· I·顏料紅 l22(Hostaperm Pink E,由 Clariant - 長:供)’實施例1 3和比較例13中使用的有機顏料為c. l · -顏料紅 177(Chromophthal Red A2B,由 Ciba SpecialtyA pigment composition was obtained in the same manner as in Example 8 except that the compound (2), the compound (3) and the compound (4) were used instead of the derivative used in Example 8.纟 2 shows the electric power consumption of the kneading f, the specific surface area according to the BET method, and the gloss value of the coated product. The BET specific surface area of the pigment compositions of Examples 9 to 11 and the glossiness value of the coated article were larger than those of Comparative Examples 8 to 11. (Examples 12 to 14 and Comparative Examples 12 to 14) The kneaded materials having the components shown in Table 2 were each kneaded under the kneading conditions shown in Table 2. These materials were separately treated in the same manner as in Example 8 to obtain a pigment composition. The organic pigment used in Example 12 and Comparative Example 12 was C·I·Pigment Red 11 (Hostaperm Pink E, from Clariant - Length: supplied). The organic pigment used in Example 1 3 and Comparative Example 13 was c. · - Pigment Red 177 (Chromophthal Red A2B, by Ciba Specialty

Chemicals Co·提供),實施例14和比較例14中使用的有 機顏料為 C· I.顏料紫 23(Sumiton Fast Violet RL Base,由 Sumi tomo Chemical Co.,Ltd·提供)。 312XP/發明說明書(補件)/95_08/95丨14255 67 200706604 實施例12到14中的用少量電功率消耗量製備的該顏料 組成物的BET法比表面積和塗覆品的光澤度值大於比較 例12到14中的值。 表2The organic pigment used in Example 14 and Comparative Example 14 was C.I. Pigment Violet 23 (Sumiton Fast Violet RL Base, supplied by Sumi tomo Chemical Co., Ltd.). 312XP/Invention Manual (Supplement)/95_08/95丨14255 67 200706604 The BET specific surface area of the pigment composition prepared by using a small amount of electric power consumption in Examples 12 to 14 and the gloss value of the coated article are larger than the comparative example. Values from 12 to 14. Table 2

實施例 比較例 表2(續) 凹印油墨塗覆 品的光澤度 %EXAMPLES Comparative Example Table 2 (continued) Gloss of gravure ink coating %

Εχ·=實施例,CEx.=比較例 312XP/發明說明書(補件)/95-08/95114255 68 200706604 在隨後的實施例之前將說明平均原始粒徑、顏料的長寬 比和比表面積以及抗蝕劑塗覆薄膜的對比度的測量方 法,以及實施例中所用的丙烯酸樹脂溶液的製備實施例。 用普通方法測量顏料的原始粒徑,其中用電子顯微鏡直 接測量原始粒子的尺寸。特別是,測量顏料原始粒子的長 轴直徑和短軸直徑,而且採用長軸直徑和短轴直徑的平均 值作為上述顏料粒子的粒徑。對於丨〇〇或更多個顏料粒 子,通過取如上獲得的粒徑的六面體的近似值單獨獲得每 個粒子的體積(重量)’採用體積平均粒徑作為平均原始粒 徑。在用透射電子顯微鏡(TEM)和掃描電子顯微鏡(sem) 的測量中,獲得了幾乎相同的結果。 通過用電子顯微鏡分別測量顏料原始粒子的長軸直徑 和短軸直徑並且根據下述方程式進行計算獲得顏料的^ 寬比。長寬比,較佳粒子的近似正方形晶形的長寬比近似 於卜 (長寬比)=(長軸直徑)/ (短軸直徑) 用BET法基於氮吸附獲得顏料粒子的比表面積。使用自 動蒸汽吸附量測量儀(「BELS0RP丨8」,由BEL Japan Inc. 提供)進行測量。 然後,芩考圖3說明使用抗蝕劑製備的塗覆膜的對比度 的測量方法。從用於液晶顯示器的背光元件(7)發出的光 透過被偏振的偏光板(6),偏振光透過塗覆在玻璃基質(5) 上的著色組成物的乾燥塗覆膜(4)並到達偏光板(3)。當偏 光板(6)的偏振面與偏光板(3)的偏振面平行時,偏光板(3) 312XP/發明說明書(補件)/95-08/95114255 69 200706604 傳輸光。當偏振面垂直時,偏光板遮斷光。然而,當 被偏光板(6 )偏振的光透過著色組成物的乾燥塗覆膜(4) 時,由於顏料粒子而出現了散射而且在部分偏振面上出現 了偏移。在該情況下,當偏光板平行時,降低了透過偏光 板(3)的光的量。當偏光板垂直時,偏光板(3)傳輸部分 光。測量被傳輸光作為偏光板上的亮度。計算偏光板平行 時的亮度和偏光板垂直時的亮度的比值(對比度)。 (對比度)=(平行亮度)/(垂直亮度) 因此,當由於著色組成物乾燥塗覆膜(4)中的顏料而出 現散射時,平行亮度降低而且垂直亮度增加。因此,對比 度降低。 形色7C度计(「BM-5A」,由Topcon提供)用作亮度計 (1),偏光板(「NPF—G1220DUN」,由 Niu〇 Denk〇Εχ·=Example, CEx.=Comparative Example 312XP/Invention Manual (Supplement)/95-08/95114255 68 200706604 The average primary particle diameter, the aspect ratio and specific surface area of the pigment, and the resistance will be explained before the subsequent examples. A method of measuring the contrast of the etchant-coated film, and a preparation example of the acrylic resin solution used in the examples. The original particle diameter of the pigment was measured by an ordinary method in which the size of the original particles was directly measured by an electron microscope. Specifically, the major axis diameter and the minor axis diameter of the pigment primary particles were measured, and the average values of the major axis diameter and the minor axis diameter were used as the particle diameter of the above pigment particles. For ruthenium or a plurality of pigment particles, the volume (weight) of each particle is individually obtained by taking an approximation of the hexahedron of the particle diameter obtained as above. The volume average particle diameter is taken as the average primary particle diameter. In the measurement by transmission electron microscopy (TEM) and scanning electron microscope (sem), almost the same results were obtained. The width ratio of the pigment was obtained by separately measuring the major axis diameter and the minor axis diameter of the pigment primary particles with an electron microscope and calculating according to the following equation. The aspect ratio, the aspect ratio of the approximate square crystal form of the preferred particles is approximately (length ratio) = (long axis diameter) / (short axis diameter) The specific surface area of the pigment particles is obtained by the BET method based on nitrogen adsorption. The measurement was carried out using an automatic vapor adsorption amount measuring instrument ("BELS0RP丨8", supplied by BEL Japan Inc.). Next, a method of measuring the contrast of a coating film prepared using a resist will be described with reference to FIG. Light emitted from the backlight element (7) for the liquid crystal display passes through the polarized polarizing plate (6), and the polarized light passes through the dried coating film (4) of the colored composition coated on the glass substrate (5) and reaches Polarizer (3). When the plane of polarization of the polarizing plate (6) is parallel to the plane of polarization of the polarizing plate (3), the polarizing plate (3) 312XP/invention specification (supplement)/95-08/95114255 69 200706604 transmits light. When the plane of polarization is vertical, the polarizing plate blocks light. However, when the light polarized by the polarizing plate (6) passes through the dried coating film (4) of the coloring composition, scattering occurs due to the pigment particles and an offset occurs on the partially polarized surface. In this case, when the polarizing plates are parallel, the amount of light transmitted through the polarizing plate (3) is lowered. When the polarizing plate is vertical, the polarizing plate (3) transmits a part of the light. The transmitted light is measured as the brightness on the polarizing plate. The ratio (contrast) of the brightness when the polarizing plates are parallel and the brightness when the polarizing plates are vertical is calculated. (Contrast) = (parallel brightness) / (vertical brightness) Therefore, when scattering occurs due to the coloring composition drying the pigment in the coating film (4), the parallel brightness is lowered and the vertical brightness is increased. Therefore, the contrast is reduced. Shaped 7C meter ("BM-5A", supplied by Topcon) used as luminance meter (1), polarizer ("NPF-G1220DUN", by Niu〇 Denk〇

Corporation提供)用作偏光板。在測量中,將具有i><icm 方孔的黑色掩膜(2)置於測量部分上,以遮斷不需要的光。 (實施例中所用的丙烯酸樹脂溶液的製備實施例) 將800份環己酮放置在反應器中,將其與引入到反應器 中的氮氣一起加熱到100t;。在同樣的溫度下向反應器滴 加60· 0份苯乙烯、60· 0份甲基丙烯酸、65· 〇份甲基丙烯 酸甲酯、65.0份丁基丙烯酸甲酯和1〇 〇份偶氮二異丁腈 的混合物超過1小時以進行聚合。滴加後,得到的混合物 在100 C進一步反應3小時。然後,添加在5〇份環己酮 中的2· 0份偶氮二異丁腈溶液。該混合物繼續反應丨小時 以獲得丙烯酸樹脂溶液,用Gpc測量,其具有約4〇,〇〇〇 312XP/發明說明書(補件)/95-08/95114255 7〇 200706604 的重均分子量。 將忒丙烯酸樹脂溶液冷卻到室溫,然後取樣部分樹脂溶 液。在180°C乾燥樣品樹脂溶液2〇分鐘並測量不揮發物 •的含量。將環己酮添加到樹脂溶液中使不揮發物的含量變 為20%,由此製備丙烯酸樹脂溶液。 (實施例15) 用轉換此 s 為(由 Asada Iron Works· Co·,LTD·提供) 近乎均勻地預混100份粗銅酞青(「T_95粗製藍」,由 則ΗΜ Τ_服⑶.,LTD.提供)、⑽份氯化納和1〇 份二伸乙甘醇5分鐘。將得到的混合物通過螺桿式計量加 料器(圖1中的計量加料部分4)供給到連續捏合機 (「MiracleK· C. K.-型 42」,由 AsadaIr〇nW〇rks. c〇., ltd.)中並揑合該混合物。連續揑合機具有12〇咖0的加 料部分螺桿直徑和八組由固定盤和旋轉盤組成的揑合部 分。在5〇rmp的主軸轉數和1〇(rc的粉碎溫度下,以2ikg/ 籲小時的揑合組成物擠出量操作連續揑合機。取出由此獲得 的被揑合材料並將其倒入7〇。〇的13〇〇份1%硫酸=液 中。保持溫度㈣該混合物丨小時,接著過濾、,用水洗務、 乾燥並粉碎,由此獲得微細銅駄青顏料。微細銅醜青顏料 具有lllmVg的比表面積。帛(電子顯微鏡德測,平 均原始粒徑為23.1_,顏料粒子全部微細細粉碎而且沒 有發現粗粒子。長寬比為L 61。 ' 然後,均勻攪拌具有包含上面獲得的微細銅酞青顏料的 以下成分的混合物’然後使用直徑為-的氧化錯珠用 312XP/發明說明書(補件)/95-08/95114255 71 200706604Provided by Corporation) as a polarizing plate. In the measurement, a black mask (2) having i><icm square holes was placed on the measuring portion to block unnecessary light. (Preparation Example of Acrylic Resin Solution Used in the Example) 800 parts of cyclohexanone was placed in a reactor, which was heated to 100 t with nitrogen gas introduced into the reactor; At the same temperature, 60. 0 parts of styrene, 60.0 parts of methacrylic acid, 65 parts of methyl methacrylate, 65.0 parts of methyl butyl acrylate and 1 part of azobis were added dropwise to the reactor. The mixture of isobutyronitrile was subjected to polymerization for more than 1 hour. After the dropwise addition, the resulting mixture was further reacted at 100 C for 3 hours. Then, a solution of 2.0 parts of azobisisobutyronitrile in 5 parts of cyclohexanone was added. The mixture was further reacted for a few hours to obtain an acrylic resin solution having a weight average molecular weight of about 4 Torr, 〇〇〇 312 XP / invention specification (supplement) / 95-08/95114255 7 〇 200706604 as measured by Gpc. The hydrazine acrylic resin solution was cooled to room temperature, and then a part of the resin solution was sampled. The sample resin solution was dried at 180 ° C for 2 minutes and the content of nonvolatiles was measured. The cyclohexanone was added to the resin solution to change the content of the nonvolatile matter to 20%, thereby preparing an acrylic resin solution. (Example 15) By converting this s (provided by Asada Iron Works Co., LTD.), 100 parts of crude copper indigo ("T_95 crude blue" was almost uniformly mixed, and then ΗΜ Τ _ (3)., LTD .)), (10) parts of sodium chloride and 1 part of diethylene glycol glycol for 5 minutes. The obtained mixture was supplied to a continuous kneader ("Miracle K· CK-type 42" by Asada Ir〇n W〇rks. c〇., ltd.) through a screw type metering feeder (metering portion 4 in Fig. 1). And kneading the mixture. The continuous kneader has a feeding portion screw diameter of 12 0 0 and eight sets of kneading portions composed of a fixed disk and a rotating disk. The continuous kneader was operated at a spindle rotation number of 5 〇 rmp and a pulverization temperature of 1 〇 (2 kgg/h), and the kneaded material thus obtained was taken out and poured into 7 〇. 13 parts of hydrazine in 1% sulfuric acid = liquid. Keep the temperature (4) the mixture 丨 hour, then filter, wash with water, dry and pulverize, thereby obtaining a fine copper phthalocyanine pigment. The fine copper ugly pigment has lllmVg Specific surface area. 帛 (electron microscopy, the average primary particle size is 23.1 _, the pigment particles are all finely pulverized and no coarse particles are found. The aspect ratio is L 61. ' Then, the uniform stirring has the fine copper obtained above. Mixture of the following ingredients of the indigo pigment 'then use oxidized wrong beads of diameter - 312XP / invention specification (supplement) / 95-08/95114255 71 200706604

Eiger 研磨機(「Minim〇del Μ-250 MKII」,由 Eiger Japan 提供)分散5小時,用5 e m篩檢程式過濾以製備藍色顏料 分散體。An Eiger mill ("Minim〇del Μ-250 MKII", supplied by Eiger Japan) was dispersed for 5 hours and filtered using a 5 e m screening procedure to prepare a blue pigment dispersion.

微細銅g太青顏料 10· 0 份 衍生物48(顏料衍生物) 1· 0份 石粦酸酯顏料分散劑 (「BYK111」,由 BYK Chemie 提供) 1· 0份 丙烯酸樹脂溶液 40· 0 份 環己酮 48· 0 份 此外’均勻攪拌和混合具有包含上面獲得的藍色著色分 散體的以下成分的混合物,然後用1 // m篩檢程式過濾以 製備鹼顯影類藍色抗蝕劑。 藍色著色分散體 45· 0 份 丙烯酸樹脂溶液 15· 0 份 三羥甲基丙烷三丙烯酸酯 9· 0份 (「NK ester ATMPT」,由 Shin-Nakamura Chemical Co., Ltd·提供) 光致聚合引發劑 2· 0份 (「 Irgacure 907」,由 Ciba Specialty Chemicals Co· 提供) 敏化劑 〇· 2份 (「EAB-F」,由 Hodogaya Chemical Co·,Ltd.提供) 環己酮 28· 8 份 (比較例15) 312ΧΡ/發明說明書(補件)/95-08/95114255 72 200706604 將100伤粗銅酞青(Γ τ—95粗製藍」,由ZHUHAI τ〇γ〇 ΙΝΚ C0·曰’ LTD·提供)、100份氯化納和1〇份二伸乙甘醇置於 容量為1〇〇〇體積份的雙臂揑合機中。在l〇〇—li(rc捏合 .該混合物曰5小時,同時混合物保持在稠密漿體狀態。研磨 後取出彳于到的混合物並將其倒入7〇。〇的1,3〇〇份丨%硫 酸溶液中。保持溫度授摔該混合物】小時,接著過滤,用 水洗滌、乾煉並粉碎,由此獲得微細銅酞青顏料。微細銅 _酞月顏料具有93m2/g的比表面積。用TEM(電子顯微鏡) 觀測,顏料粒子全部被微細粉碎而且沒有發現粗粒子。然 而,平均原始粒徑為72· 3nm,長寬比為1· 75。 以與貝鈀例15同樣的方式使用上面獲得的微細銅酞青 顏料製備鹼顯影類藍色抗蝕劑。 (實施例16) 將含有1 00 刀啥击酞酉同(qUin〇phthai〇ne)顏料(c· I· 顏料頁138,「?&11〇1;〇1¥611簡1(〇961111)」,由^31?提供)、 # 3, 000份氯化鈉和7〇〇份二伸乙甘醇的揑合組成物供給到 與實施例15中所用的相同的揑合機中,並在5〇rpm的主 轴轉數和11(TC的研磨溫度下,以25kg/小時的揑合組成 物擠出量揑合該組成物。以與實施例15同樣的方式淨 =、過濾、乾燥和粉碎由此獲得的被揑合材料以獲得微細 喹諾酞酮顏料。該微細喹諾酞酮顏料具有115m2/g的比表 面積。用TEM(電子顯微鏡)觀測,平均原始粒徑為 33· 2nm’顏料粒子全部被細細粉碎而且沒有發現粗粒子。 長寬比為1. 53。 312XP/發明說明書(補件)/95-08/95114255 73 200706604 ^後均句攪拌具有包含上面獲得的微細喹諾酞酮顏料 的=下成刀的混合物,然後以與實施例丨5同樣的方式將 八刀_政和過/慮以獲得黃色顏料分散體。此外,以與實施例 15,同樣的方式使用上面獲得的黃色顏料分散體製備鹼顯 影類黃色抗餘劑。 微細喹諾酞_顏料 1 〇 〇份 衍生物3 9 (顏料衍生物) 1 0份 填酸酯顏料分散劑 1. 0份 40. 0 份 48. 0 份 (BYK111」’由 βγΚ Chemie 提供) 丙烯酸樹脂溶液 環己酮 (比較例16) 將100份喧諾酞_顏料(c.丨.顏料黃m,「Paii〇t〇i YellowK0961HD」,由BASF提供)、3〇〇〇份氯化鈉和7〇〇份 二伸乙甘醇置於容量為1000體積份的雙臂揑合機中。在 • 100-11G°C揑合該混合物6小時,同時混合物保持在稠穷 漿體狀態。研磨後,取出得到的混合物並將其倒入7〇 = 的1 ’ 300份1 %硫酸溶液中。保持溫度攪拌該混合物!小 時,接著過濾,用水洗滌、乾燥並粉碎,由此獲得微細喹 諾酞酮顏料。微細喹諾酞酮顏料具有95m2/g的比表面積。 用TEM(電子顯微鏡)觀測,顏料粒子全部被微細粉碎而且 沒有發現粗粒子。然而,平均原始粒徑為82 5nm,長寬 微細啥諾酞 以與實施例1 β同樣的方式使用上面獲得的 312ΧΡ/發明說明書(補件)/95-08/95114255 74 200706604 酉同顏料製備驗顯影類黃色抗餘劑。 (實施例17) 將含有1 0 〇份二酮义* ,「觀_ RED B-CF,、Γ (C. L 顏料紅 254Fine copper g toffee pigment 10·0 part derivative 48 (pigment derivative) 1·0 part of rhodium phthalate pigment dispersant (“BYK111”, supplied by BYK Chemie) 1·0 part acrylic resin solution 40·0 parts Cyclohexanone 48·0 parts Further, a mixture having the following components containing the blue colored dispersion obtained above was uniformly stirred and mixed, and then filtered using a 1 // m screening procedure to prepare an alkali-developing blue resist. Blue coloring dispersion 45·0 parts Acrylic resin solution 15·0 parts Trimethylolpropane triacrylate 9·0 parts (“NK ester ATMPT”, supplied by Shin-Nakamura Chemical Co., Ltd.) Photopolymerization 2 parts of the initiator ("Irgacure 907", supplied by Ciba Specialty Chemicals Co.) sensitizer 〇 2 parts ("EAB-F", supplied by Hodogaya Chemical Co., Ltd.) Cyclohexanone 28·8 (Comparative Example 15) 312ΧΡ/Invention Manual (supplement)/95-08/95114255 72 200706604 100-injured blister copper indigo (Γτ-95 crude blue) by ZHUHAI τ〇γ〇ΙΝΚ C0·曰' LTD· Provided, 100 parts of sodium chloride and 1 part of diethylene glycol were placed in a two-arm kneader having a capacity of 1 part by volume. The mixture was kneaded for 5 hours while the mixture was kept in a dense slurry state. After grinding, the resulting mixture was taken out and poured into 7 〇. 1,3 parts of 〇 In the % sulfuric acid solution, the mixture was allowed to fall for a few hours, followed by filtration, washing with water, drying and pulverization, thereby obtaining a fine copper indigo pigment. The fine copper_yield pigment had a specific surface area of 93 m 2 /g. (Electron Microscope) It was observed that all the pigment particles were finely pulverized and no coarse particles were observed. However, the average primary particle diameter was 72·3 nm, and the aspect ratio was 1.75. The same procedure as that used in the case of Palladium 15 was used. A fine copper phthalocyanine pigment is used to prepare an alkali-developing blue resist. (Example 16) A pigment containing 100 knives (qUin〇phthai〇ne) will be contained (c·I·pigment page 138, "?&;11〇1;〇1¥611简1(〇961111)", supplied by ^31?), #3,000 parts of sodium chloride and 7 parts of diethylene glycol, kneaded composition supplied and implemented In the same kneading machine used in Example 15, and the spindle rotation speed at 5 rpm and the grinding temperature of 11 (TC) The composition was kneaded at a kneading composition extrusion amount of 25 kg / hr. The kneaded material thus obtained was net-filtered, filtered, dried and pulverized in the same manner as in Example 15 to obtain a fine quinolone pigment. The fine quinolone pigment had a specific surface area of 115 m 2 /g. The average primary particle diameter was 33·2 nm as observed by TEM (electron microscopy). The pigment particles were all finely pulverized and no coarse particles were found. 53. 312XP/Invention Manual (Supplement)/95-08/95114255 73 200706604 ^After the sentence is stirred, the mixture having the lower knives containing the fine quinolone pigment obtained above, and then with the example 丨5 In the same manner, a yellow pigment dispersion was obtained in the same manner as in Example 15. Further, an alkali-developing yellow anti-retaining agent was prepared in the same manner as in Example 15 using the yellow pigment dispersion obtained above. _Pigment 1 Hydrazine derivative 3 9 (Pigment derivative) 10 parts of sulphonate pigment dispersant 1. 0 parts 40. 0 parts 48. 0 parts (BYK111" 'provided by βγΚ Chemie) Acrylic resin solution Ketone (Comparative Example 1 6) 100 parts of 喧 酞 颜料 pigment (c. 丨. pigment yellow m, "Paii〇t〇i YellowK0961HD", supplied by BASF), 3 parts of sodium chloride and 7 parts of diethylene glycol The alcohol was placed in a two-arm kneader having a capacity of 1000 parts by volume. The mixture was kneaded at 100-11 G ° C for 6 hours while the mixture was kept in a state of viscous slurry. After grinding, the resulting mixture was taken out and poured into it. 7 〇 = 1 '300 parts in 1% sulfuric acid solution. Stir the mixture while maintaining the temperature! In the next, it was filtered, washed with water, dried and pulverized, whereby a fine quinolone pigment was obtained. The fine quinolone pigment has a specific surface area of 95 m 2 /g. When observed by TEM (electron microscopy), all the pigment particles were finely pulverized and no coarse particles were found. However, the average primary particle diameter was 82 5 nm, and the length and width micron oxime was used in the same manner as in Example 1 β using the 312 ΧΡ/invention specification (supplement)/95-08/95114255 74 200706604 Developed yellow anti-surplus agent. (Example 17) will contain 10 〇 diketone sense*, "View _ RED B-CF, Γ (C. L Pigment Red 254

Co 描供〕 」由 Clba Specialty Chemicals = M、)、2, _❾氯化納和⑽份二伸乙甘醇的捏合植 成物供給到與實施例15中所用沾 、、 5〇rPm的主軸轉數和6rr:斤用的相同的揑合機中,並在 揑合组成物//Γ的研磨溫度下,以2啦/小時的 方式淨化I里揑合該組成物。以與實施例15同樣的 得^ 乾燥和粉碎由此獲得的被揑合材料以獲 且 4枓。该微細二酮吡咯並吡咯顏料 心料m g的比表面積1 TEM(電子顯微鏡)觀測,平 心⑽,顏料粒子全部被細細粉碎而且沒 有發現粗粒子。長寬比為1.61。 ,後,均W拌具有包含上面獲得的微細二酮鱗並吼 咯顏料的以下成分的、、日人4 方六、蔣JL八批 此^物,然後以與實施例15同樣的 二、/、刀月和過濾以獲得紅色顏料分散體。此外,以與 :::"5同樣的方式使用上面獲得的紅色顏料分散體製 備驗顯影類紅色抗蝕劑。 微細二酮吡咯並吡咯顏料 衍生物49(顏料衍生物) 磷酸酯崩料分散劑 10· 0 份 1· 0份 (「BYK111」’由 BYK Chemie 提供) 丙烯酸樹脂溶液 1· 0份 40· 0 份 48· 0 份 環己酮 312XP/發明說明書(補件)/95-08/95114255 75 200706604 (比較例17) 將loo份二酮吡咯並吡咯顏料(c.丨·顏料紅254,「丨rgaph〇r RED^B-CFv ^ Ciba Specialty Chemicals Co. ^^).2,000 份氣化納和230份二伸乙甘醇置於容量為1〇〇〇體積份的 雙臂揑合機中。在65_肌揑合該混合物6小時,同時混 合物保持在稠密漿體狀態。研磨後,取出得到的混合物並 將其倒人70 C的20, GGG份1%硫gB液中。保持溫度授 拌該混^物H、時’接著_,用水絲、乾燥並粉碎, 由此獲得微細二酮吡咯並吡咯顏料。微細二酮吡咯並吡咯 顏料具有105mVg㈤比表面積。用TEM(電子顯微鏡)觀測, 顏料粒子全部被細細粉碎而且沒有發絲粒子。然而,平 均原始粒徑為69.5nm,長寬比為181。 以與實施例Π同樣的方式使用上面獲得的微細二嗣吼 咯並吡咯顏料製備鹼顯影類紅色抗蝕劑。 (實施例18) 將含有1〇〇份粗製二崎啡紫色顏料(Sumit〇n F时 = ^Base ’ 由 Sumitomo Chemical Co·,Ltd·提供)、1,000 份氯化鈉卩15〇份二伸乙甘醇的揑合組成物供給到與實 施例15中所用的相同的揑合機中,並在5〇rpm的主軸轉 數^ iooc的研磨溫度下’卩22kg/小時的捏合組成物擠 出!揑合該組成物。以與實施例15同樣的方式淨化、過 =、乾煉和粉碎由此獲得的被揑合材料以獲得微細二哼畊 I色顏料。該微細二,畊紫色顏料具有14GmVg的比表面 312XP/發明說明書(補件)/95-08/95114255 76 200706604 子”、員从叙)硯測’平均原始粒徑為30. 3nm,顏 料粒子全部被細知#访工 m顏 叔碎而且沒有發現粗粒子。長寬比為 1 · b d 〇 〜 然後,均句授拌具有包含上面獲得的微細二十 料的以下成分的混合物,然後以與實施例15同樣的方二 將其分散和過^獲得紫色誠分散體。此外,以與實施 例15同樣的方式使用上面獲得的紫色顏料分散體製備驗Co-drawing] The kneaded plant of Clba Specialty Chemicals = M,), 2, _ ❾ ❾ ❾ and (10) parts of diglycol was supplied to the spindle of 5 〇 rPm used in Example 15 The composition was kneaded in the same kneading machine as 6 rr: kg, and at a grinding temperature of the kneaded composition // ,, in a manner of 2 la / h. The kneaded material thus obtained was dried and pulverized in the same manner as in Example 15 to obtain 4 Å. The specific surface area of the fine diketopyrrolopyrrole pigment m g was observed by TEM (electron microscopy), and the center (10), the pigment particles were all finely pulverized and no coarse particles were found. The aspect ratio is 1.61. Then, all of the following components having the following components of the fine diketone scale fluorene pigment obtained above were collected, and the same batch of the same as in Example 15 was used. , knife month and filtration to obtain a red pigment dispersion. Further, the developed red resist was prepared in the same manner as ::: " 5 using the red pigment dispersion obtained above. Fine diketopyrrolopyrrole pigment derivative 49 (pigment derivative) Phosphate fragmentation dispersant 10·0 parts 1·0 parts (“BYK111”' is supplied by BYK Chemie) Acrylic resin solution 1·0 parts 40·0 parts 48·0 parts of cyclohexanone 312XP/invention specification (supplement)/95-08/95114255 75 200706604 (Comparative Example 17) loo a diketopyrrolopyrrole pigment (c. 丨·Pigment Red 254, “丨rgaph〇 r RED^B-CFv ^ Ciba Specialty Chemicals Co. ^^). 2,000 parts of gasified sodium and 230 parts of diethylene glycol were placed in a two-arm kneader with a capacity of 1 part by volume. The mixture was kneaded for 6 hours while the mixture was kept in a dense slurry state. After grinding, the resulting mixture was taken out and poured into a 70 C 20 g, GGG portion 1% sulfur gB solution. The mixture was kept at a temperature. Then, 'continued _, water-filament, dried and pulverized, thereby obtaining a fine diketopyrrolopyrrole pigment. The fine diketopyrrolopyrrole pigment has a specific surface area of 105 mVg (v). The TEM (electron microscope) observed that the pigment particles were all fine. Crushed without hair particles. However, the average primary particle size was 69. 5 nm, aspect ratio was 181. An alkali-developing red resist was prepared in the same manner as in Example 使用 using the fine di-pyrrolopyrrole pigment obtained above (Example 18) 1 part of crude 2 A kneading composition of a succinimide violet pigment (Sumit〇n F = ^Base 'provided by Sumitomo Chemical Co., Ltd.), 1,000 parts of sodium chloride 卩15 parts of diethylene glycol, and the same example In the same kneading machine used in the above, the kneaded composition of '卩22 kg/hr was extruded at a grinding temperature of 5 rpm of the spindle speed of iooc! The composition was kneaded. In the same manner as in Example 15. Purification, over-, dry-drying and pulverization of the kneaded material thus obtained to obtain a fine diterpene I color pigment. The fine second, ploughed purple pigment has a specific surface of 14 GmVg 312XP / invention specification (supplement) / 95-08 /95114255 76 200706604 "", the staff from the Syrian) speculation that the average particle size of 30.3 nm, the pigment particles are all well-known # interview m Yan Shu broken and found no coarse particles. The aspect ratio is 1 · bd 〇 ~ Then, a mixture having the following components containing the fine twentieth material obtained above is mixed, and then dispersed and passed in the same manner as in Example 15 to obtain a purple dispersion. body. Further, the preparation of the purple pigment dispersion obtained above was used in the same manner as in Example 15.

顯影類紫色抗勉劑。 10· 0 份 1· 〇份 1· 〇份 40· 0 份 48· 〇 份 微細二哼啡紫色顏料 衍生物48(顏料衍生物) 鱗酸酿顏料分散劑 (BYK111」,由 BYK chemie 提供) 丙烯酸樹脂溶液 環己酉同 (比較例18) 將1〇〇份粗製二崎讲紫色顏料(SumitonFast Vi〇iet虬Developed purple anti-caries agent. 10·0 parts 1· 〇1· 〇 40·0 parts 48· 微 微 微 哼 紫色 紫色 紫色 紫色 紫色 48 ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( ( BY BY Resin solution is the same as in the above (Comparative Example 18) 1 part of crude akisaki purple pigment (SumitonFast Vi〇iet虬

Base,由 Sumitomo Chemical Co.,Ltd·提供)、1,0〇〇 份 氣化鈉和150份二伸乙甘醇置於容量為1〇〇〇體積份的雙 臂揑合機中。在100 —11 〇。〇揑合該混合物5小時,同時混 合物保持在稠密漿體狀態。研磨後,取出得到的混合物2 將其倒入70t的1 0, 000份1%硫酸溶液中。保持溫度攪 拌該混合物1小時,接著過濾,用水洗滌、乾燥並粉碎, 由此獲得微細二哼啡紫色顏料。微細二哼啡紫色顏料具有 93m2/g的比表面積。用TEM(電子顯微鏡)觀測,顏料粒子 312XP/發明說明書(補件)/95-08/95114255 77 200706604 全部被細細粉碎而且沒有發現粗粒子。然而, 徑為59.5nm,長寬比為拉 以與實施例18同樣的方式使用上面獲得的微細二 -紫色顏料製備鹼顯影類紫色抗蝕劑。 (實施例19) 將含有100份粗製銅酞青顏料(「τ_95粗製該」,由 翻Αί τ請1财⑶.,ltd.提供)、_份氣化;;、⑽ 份二伸乙甘醇和5份松香樹脂作為樹脂的捏合組成物供 給到與實施例15中所用的相同的揑合機中,並在5〇rpm 的主軸轉數和9(rc的研磨溫度下,以22kg/小時的揑合組 成物擠出量揑合該組成物。以與實施例15同樣的方式淨 化、過濾、乾燥和粉碎由此獲得的被揑合材料以獲得微細 粗銅酞青顏料。該微細粗銅酞青顏料具有i28mVg的比表 積用TEM(黾子顯微鏡)觀測,平均原始粒徑為 21. lnm,顏料粒子全部被細細粉碎而且沒有發現粗粒子。 ⑩長寬比為1. 54。 然後,均勻攪拌具有包含上面獲得的微細粗銅酞青顏料 的以下成分的混合物,然後以與實施例15同樣的方式將 其分散和過濾以獲得藍色顏料分散體。此外,以與實施例 15同樣的方式使用上面獲得的藍色顏料分散體製備鹼顯 - 影類藍色抗钱劑。 微細粗銅酞青顏料 10· 〇份 竹生物4 8 (顏料衍生物) 1 0份 碟酸酯顏料分散劑 312XP/發明說明書(補件)/95·〇8/95 i 14255 78 200706604 1· 0份 40. 0 份 48. 0 份 (「BYK111」,由 BYK Chemie 提供) 丙烯酸樹脂溶液 環己酮 (比較例19) 將100伤粗銅g太青顏料(「T-95粗製藍」,由zhujja丨τογο INK C0.,LTD.提供)、60〇份氯化鈉、1〇〇份二伸乙甘醇 和5份松香樹脂作為樹脂置於容量為丨〇〇〇體積份的雙臂 揑合機中。在揑合該混合物5小時,同時混合物保 持在稠密漿體狀態。研磨後,取出得到的混合物並將其倒 入70°C的1,300份1%硫酸溶液中。保持溫度攪拌該混合 物1小時,接著過濾’帛水洗滌、乾燥並粉碎,由此獲得 微細粗銅酞青顏料。微細粗銅酞青顏料具有97mVg的比 表面積。肖TEM(電子顯微鏡)觀測,顏料粒子全部被細細 粉碎而且沒有發現粗粒子。然@,平均原始粒徑為 68. 9nm,長寬比為1. 71。Base, supplied by Sumitomo Chemical Co., Ltd., 1,0 parts of sodium carbonate and 150 parts of ethylene glycol were placed in a two-arm kneader having a volume of 1 part by volume. At 100 — 11 〇. The mixture was kneaded for 5 hours while the mixture remained in a dense slurry state. After grinding, the resulting mixture 2 was taken out and poured into 70 tons of 1 000 parts of a 1% sulfuric acid solution. The mixture was stirred at a temperature for 1 hour, followed by filtration, washing with water, drying and pulverization, whereby a fine diterpene violet pigment was obtained. The fine diterpene violet pigment has a specific surface area of 93 m 2 /g. Observation by TEM (electron microscopy), the pigment particles 312XP/invention specification (supplement)/95-08/95114255 77 200706604 were all finely pulverized and no coarse particles were found. However, the diameter was 59.5 nm, and the aspect ratio was pulled. In the same manner as in Example 18, an alkali-developing-type purple resist was prepared using the fine di-purple pigment obtained above. (Example 19) 100 parts of crude copper indigo pigment ("τ_95 crude", supplied by 1 Α 1 财 (3).,ltd.), _ part of gasification;;, (10) part of diethylene glycol and 5 parts of rosin resin was supplied as a kneaded composition of the resin to the same kneader used in Example 15, and was kneaded at a spindle rotation speed of 5 rpm and a grinding temperature of 9 (rc) at 22 kg/hr. The composition was kneaded by the amount of extrusion. The kneaded material thus obtained was purified, filtered, dried and pulverized in the same manner as in Example 15 to obtain a fine crude copper indigo pigment. The fine crude copper indigo pigment had a ratio of i28 mVg. The average original particle size was observed to be 21. lnm, and the pigment particles were all finely pulverized and no coarse particles were found. 10 The aspect ratio was 1.54. Then, the uniform stirring had the above obtained A mixture of the following components of the fine copper phthalocyanine pigment was dispersed and filtered in the same manner as in Example 15 to obtain a blue pigment dispersion. Further, the blue pigment obtained above was used in the same manner as in Example 15. Minute Preparation of alkali-shadow blue anti-money agent. Micro-copper copper indigo pigment 10·〇竹竹4 8 (pigment derivative) 10 parts dish ester pigment dispersant 312XP/invention manual (supplement)/95 ·〇8/95 i 14255 78 200706604 1·0 parts 40. 0 parts 48. 0 parts (“BYK111”, supplied by BYK Chemie) Acrylic resin solution cyclohexanone (Comparative Example 19) 100% of blister copper g-green pigment ("T-95 crude blue", supplied by zhujja丨τογο INK C0., LTD.), 60 parts of sodium chloride, 1 part of diethylene glycol and 5 parts of rosin resin as a resin. 〇〇 Volume of the double-arm kneader. The mixture was kneaded for 5 hours while the mixture was kept in a dense slurry state. After grinding, the resulting mixture was taken out and poured into 1,300 parts of 1% sulfuric acid at 70 °C. In the solution, the mixture was stirred at a temperature for 1 hour, followed by filtration, washing with water, drying and pulverization, thereby obtaining a fine crude copper indigo pigment. The fine crude copper indigo pigment had a specific surface area of 97 mVg. Observed by TEM (electron microscopy), The pigment particles were all finely pulverized and found not 5。 The average particle size is 68. 9nm, the aspect ratio is 1. 71.

以與實施例15同樣的方式使用上面獲得的微細粗銅敵 青顏料製備鹼顯影類藍色抗蝕劑。 (實施例20) 將含有100份粗銅酿青顏料(「τ_95粗製藍」,由删脇 T_INKCO·,LTD·提供)、600份氯化納、1〇〇份二伸乙 甘醇和5份衍生物51(顏料衍生物)的揑合組成物供給到 與實施例15中所用的相同的揑合機中,並在5Grpm的主 轴轉數和100°c的研磨溫度下,卩22kgAj、時的揑合纽成 物擠出量揑合該組成物。以與實施例15㈣的方式淨 312XP/發明說明書(補件)/95·08/95114255 79 200706604 J 匕、;廣 Λ iA l^r ^ 卞粉碎由此獲得的被揑合材料以獲得微細 而二1顏料。該微細粗銅酞青顏料具有132m2/g的比表 =。用TEM(電子顯微鏡)觀測,平均原始粒徑為 nm顏料粒子全部被細細粉碎而且沒有發現粗粒子。 長覓比為1. 5〇。 …、後均勻攪拌具有包含上面獲得的微細粗銅酞青顏料 111成分的混合物’然後以與實施例15同樣的方式將 八 '政和過濾以獲得藍色顏料分散體。此外,以與實施例 15 ,同樣的方式使用上面獲得的藍色顏料分散體製備驗顯 影類藍色抗钱劑。 微細粗銅酞青顏料 10· 0 份 衍生物48(顏料衍生物) 1· 0份 填酸酯顏料分散劑 (「BYK111」,由 BYK Chemie 提供) 1· 0份 丙烯酸樹脂溶液 40· 0 份 環己酉同 48· 0 份 (比較例20) 將100份粗銅酞青顏料(「T-95粗製藍」,由ZHUHAIT〇Y〇 INK CO.,LTD·提供)、600份氯化鈉、1〇〇份二伸乙甘醇 和5份衍生物51(顏料衍生物)置於容量為1〇〇〇體積份的 雙臂揑合機中。在100°C揑合該混合物5小時,同時混合 物保持在稠密漿體狀態。研磨後,取出得到的混合物並將 其倒入7 0 C的1,3 0 0份1 %硫酸溶液中。保持溫度授摔兮 混合物1小時,接著過滤,用水洗滌、乾燥並粉碎,由此 312XP/發明說明書(補件)/95-08/95114255 80 200706604 獲得微細粗銅酞青顏料。微細粗銅酞青顏料具有99m2/g 的比表面積。用TEM(電子顯微鏡)觀測,顏料粒子全部被 ,細細粉碎而且沒有發現粗粒子。然而,平均原始粒徑為 - 66· 3nm,長寬比為丨· 69。 以與實施例15同樣的方式使用上面獲得的微細粗銅醜 青顏料製備鹼顯影類藍色抗蝕劑。 表3顯示了實施例15到2 0和比較例15到2 0中獲得的 微細顏料的比表面積、平均原始粒徑和長寬比的測量結 •果。 、° 對於實施例15到20和比較例15到20中獲得的各個抗 名虫劑’製備三個膜厚度不同的塗覆基質。測量每個膜厚度 和每個對比度。用原始相關法由上述三個塗覆基質的資料 得出在2//m膜厚度的對比度。通過改變所使用旋塗機的 轉數將抗姓劑施力口到基質上,以使製備的每個塗覆基質具 有約l//m的幹膜厚度,然後在熱空氣箱中在8〇°C將其乾 Φ燥3 0分鐘。 通過使用實施例15到20中獲得的抗蝕劑製備的塗覆基 質的對比度高於使用比較例15到20中獲得的抗蝕劑製備 的塗覆基質的對比度。 表3An alkali-developing blue resist was prepared in the same manner as in Example 15 using the fine crude copper-based pigment obtained above. (Example 20) 100 parts of crude copper green pigment ("τ_95 crude blue", supplied by T_INKCO·, LTD.), 600 parts of sodium chloride, 1 part of diethylene glycol and 5 parts of derivatives were contained. The kneaded composition of 51 (pigment derivative) was supplied to the same kneader as used in Example 15, and at a spindle rotation speed of 5 G rpm and a grinding temperature of 100 ° C, a kneading of 22 kg of Aj was obtained. The composition was kneaded by the amount of extrusion. In the manner of Example 15 (4), the net 312XP/invention specification (supplement)/95·08/95114255 79 200706604 J 匕,; 广Λ iA l^r ^ 卞 pulverize the kneaded material thus obtained to obtain fineness pigment. The fine crude copper indigo pigment has a ratio of 132 m2/g. Observation by TEM (electron microscopy), the average primary particle diameter of the nm pigment particles was finely pulverized and no coarse particles were found. The long 觅 ratio is 1. 5〇. After that, the mixture having the composition of the fine crude copper indigo pigment 111 obtained above was uniformly stirred, and then filtered and filtered to obtain a blue pigment dispersion in the same manner as in Example 15. Further, an anthraquinone-like blue anti-money agent was prepared in the same manner as in Example 15 using the blue pigment dispersion obtained above. Fine copper copper indigo pigment 10·0 parts Derivative 48 (pigment derivative) 1·0 part of the sulphonate pigment dispersing agent (“BYK111”, supplied by BYK Chemie) 1·0 part acrylic resin solution 40·0 part ring 48同48·0 parts (Comparative Example 20) 100 parts of crude copper indigo pigment ("T-95 crude blue", supplied by ZHUHAIT〇Y〇INK CO., LTD.), 600 parts of sodium chloride, 1〇〇 The diethylene glycol and 5 parts of the derivative 51 (pigment derivative) were placed in a two-arm kneader having a volume of 1 part by volume. The mixture was kneaded at 100 ° C for 5 hours while the mixture was maintained in a dense slurry state. After the milling, the resulting mixture was taken out and poured into a 70 ° solution of 1,300 parts of 1% sulfuric acid. The mixture was allowed to wrestle for 1 hour, then filtered, washed with water, dried and pulverized, thereby obtaining a fine crude copper indigo pigment from 312XP/Invention Manual (Supplement)/95-08/95114255 80 200706604. The fine crude copper indigo pigment has a specific surface area of 99 m 2 /g. When observed by TEM (electron microscopy), all the pigment particles were finely pulverized and no coarse particles were found. However, the average primary particle diameter is -66·3 nm, and the aspect ratio is 丨·69. An alkali-developing blue resist was prepared in the same manner as in Example 15 using the fine crude copper ugly pigment obtained above. Table 3 shows the measurement results of the specific surface area, the average primary particle diameter, and the aspect ratio of the fine pigments obtained in Examples 15 to 20 and Comparative Examples 15 to 20. Three coated substrates having different film thicknesses were prepared for each of the antifungal agents obtained in Examples 15 to 20 and Comparative Examples 15 to 20. Each film thickness and each contrast was measured. The contrast at a film thickness of 2//m was obtained from the data of the above three coated substrates by the original correlation method. The anti-surname agent is applied to the substrate by changing the number of revolutions of the spin coater used so that each of the prepared coated substrates has a dry film thickness of about 1//m, and then 8 在 in a hot air tank. Dry it at °C for 30 minutes. The contrast ratio of the coating substrate prepared by using the resists obtained in Examples 15 to 20 was higher than that of the coating substrates prepared using the resists obtained in Comparative Examples 15 to 20. table 3

Ex. 15 Ex. 16 Ex. 17 Ex. 18 Ex. 19 Ex. 20 顏料 藍 黃 紅 紫 藍 藍 顏料1 顏料1 顏料1 顏料1 顏料2 顏料1 比表面積(m2/g) 111 115 122 140 128 132 平均原始粒徑(nm) 23. 1 33.2 35.2 30.3 21. 1 20.2 長寬比 1. 61 1.53 1. 61 1.63 1.54 1.50 對比度 6,500 7, 200 7, 500 6, 100 6,800 6,900 312XP/發明說明書(補件)/95-08/95114255 81 200706604Ex. 15 Ex. 16 Ex. 17 Ex. 18 Ex. 19 Ex. 20 Pigment Blue Yellow Red Violet Blue Pigment 1 Pigment 1 Pigment 1 Pigment 1 Pigment 2 Pigment 1 Specific Surface Area (m2/g) 111 115 122 140 128 132 Average Original particle size (nm) 23. 1 33.2 35.2 30.3 21. 1 20.2 Aspect ratio 1.61 1.53 1. 61 1.63 1.54 1.50 Contrast 6,500 7, 200 7, 500 6, 100 6,800 6,900 312XP/Invention manual (supplement) /95-08/95114255 81 200706604

Ex.=實施例 表3(續)Ex.=Examples Table 3 (continued)

CEx.=比較例 圖式簡單說明】 顏料 比表面積(m2/g) 平均原始粒徑(nm) 長寬比 對比度CEx.=Comparative example: Simple description of the formula] Pigment specific surface area (m2/g) Average original particle size (nm) Aspect ratio Contrast

具體例的剖面 圖1是顯示用在本發明中的連續揑合機 側視圖。 圖2顯示了圖1所示連續揑合機之具體例所採用的固定 盤和旋轉盤的前視圖和後視圖。在圖2中,(a)是*胪^ 形(cavity-sector-shaped)固定盤,(b)是空腔扇形旋^ 盤,(c)是空腔玫瑰形(cavity 一 rose—shaped)固定盤,(幻 是空腔玫瑰形旋轉盤,(e)是空腔臼形 (cavity-mortar-shaped)固定盤,(〇是空腔臼形旋轉盤。 圖3是用於測量對比度的測量裝置示意圖。 【主要元件符號說明】 1 加料部分 2 揑合部分 3 出料部分 4 計量加料器部分 10 連續揑合機 3_發明說明書(補件)/95-08/95114255 82 200706604 11 外殼 12 螺旋桿 21 固定盤 21a 空腔扇形固定盤 21c 空腔玫瑰形固定盤 21e 空腔臼形固定盤 22 揑合圓筒 23 旋轉盤 23b 空腔扇形旋轉盤 23d 空腔玫瑰形旋轉盤 23f 空腔臼形旋轉盤 24 螺桿 41 原料漏斗 42 螺旋加料器 43 連接圓柱體 44 中間圓柱體 111 原料入口 121 傳動軸 122 螺旋形翅片 211 活動裝配孔 212 空腔 231 裝配孔 232 空腔 (1) 免度计 312XP/發明說明書(補件)/95-08/95114255 83 200706604 (2) 黑色掩膜 (3) 偏光板 (4) 乾燥塗覆膜 (5) 玻璃基質 (6) 偏光板 (7) 背光元件Cross section of a specific example Fig. 1 is a side view showing a continuous kneader used in the present invention. Fig. 2 is a front view and a rear view showing a fixed disk and a rotary disk employed in a specific example of the continuous kneading machine shown in Fig. 1. In Fig. 2, (a) is a cavity-sector-shaped fixed disk, (b) is a cavity fan-shaped disk, and (c) is a cavity rose-shaped fixed. Disk, (phantom is a cavity rose-shaped rotating disk, (e) is a cavity-mortar-shaped fixed disk, (〇 is a cavity-shaped rotating disk. Figure 3 is a measuring device for measuring contrast Schematic diagram [Main component symbol description] 1 Feeding section 2 Kneading section 3 Discharging section 4 Metering feeder section 10 Continuous kneading machine 3_Invention manual (supplement)/95-08/95114255 82 200706604 11 Housing 12 auger 21 fixed Disk 21a cavity sector-shaped fixed disk 21c cavity rose-shaped fixed disk 21e cavity-shaped fixed disk 22 kneading cylinder 23 rotating disk 23b cavity sector-shaped rotating disk 23d cavity rose-shaped rotating disk 23f cavity-shaped rotating disk 24 screw 41 material funnel 42 screw feeder 43 connection cylinder 44 intermediate cylinder 111 material inlet 121 drive shaft 122 spiral fin 211 movable assembly hole 212 cavity 231 assembly hole 232 cavity (1) exemption meter 312XP / invention manual ( Patch) /9 5-08/95114255 83 200706604 (2) Black mask (3) Polarizing plate (4) Dry coating film (5) Glass substrate (6) Polarizing plate (7) Backlight component

312XP/發明說明書(補件)/95-08/95114255312XP / invention manual (supplement) / 95-08/95114255

Claims (1)

200706604 十、申請專利範圍·· 人1· 一 =顏料組成物之製法,該製法包括用連續揑合機揑 :包3有機顏料、水溶性無機鹽、水溶性有機液體及樹 月曰=/ b δ物该連續揑合機包括傳動軸、環形固定盤、與 固定盤同心且整個繞傳動軸的軸旋轉的旋轉盤及在固定 ‘和旋轉盤之間的間隙中形成的粉碎空間。 匕2·如中請專利範圍第!項之製法,其中該樹脂係松香樹 脂。 3. 一種顏料組成物之製法,該製法包括 =有,料衍生物训生物或三讲衍生物、= Ρ水&性無機鹽及水溶性有機液體 =含有選自隨亞胺基曱基、胺基、績酸基 :般Γ個取代基’該連續揑合機包括傳動軸、環形固 =二Π:同:且整個繞傳動軸的軸旋轉的旋轉盤及 在固疋盤和㈣盤之間的間隙中形成的粉碎空間。 2如=專利範圍第丨項之製法,其中有機 啉顏料、二萘嵌苯顏料、莊 一弓丨木 硫毅藍顏料、二料叫並❸各顏料、 蒽酉昆顏料。 ~4、^_顏料、㈣顏料或散 5.-種用於彩色遽^的著色, 樹脂、其先質或其混合物的顏;,::有透明 包含用連續揑合機揑合包=及顏^其中該顏料 溶性有機液體的混合物 、二;'、、水洛性無機鹽和水 物而獲件的微細有機顏料,該連續揑 312ΧΡ/發明說明書(補件)/95·08/95114255 85 200706604 動;:的軸!形固定盤、與固定盤同心且整個繞傳 中形成的粉^空^轉盤及在固定盤和旋轉盤之間的間隙 中,每! 利乾圍第5項之著色組成物’其中在混合物 機鹽和0·1 1至,"°重量份的水溶性無 7 Λ由I份的水溶性有機液體。 顏料”id 圍第5項之著色組成物,其中該含有機 到有機液體的綱係在10 掩中、二專利圍第5項之著色組成物,其中該含有機 脂:水☆性热機鹽和水溶性有機液體的混合物更包含樹 :如申請專利範圍第5項之著色組成物,其中該含有機 >、枓、水洛性無機鹽和水溶性有機液體的混合物更 料衍生物。 _ — 10·種形色濾光片,其包含由申請專利範圍第5項之 著色組成物所形成的彩色濾光片片段。 、 312XP/發明說明書(補件)/95-08/95114255 86200706604 X. Patent application scope · · Person 1 · A = method for preparing pigment composition, which comprises kneading with a continuous kneader: package 3 organic pigment, water-soluble inorganic salt, water-soluble organic liquid and tree 曰 = / b δ The continuous kneader includes a drive shaft, an annular fixed disk, a rotary disk that is concentric with the fixed disk and rotates around the axis of the drive shaft, and a pulverizing space formed in a gap between the fixed 'and the rotating disk.匕2·Please ask for the scope of patents! The method of the invention, wherein the resin is a rosin resin. 3. A method for preparing a pigment composition, comprising: a compound, a derivative derivative or a three-speaking derivative, a hydrazine & an inorganic salt, and a water-soluble organic liquid; Amine, acid base: like a substituent 'The continuous kneader includes a drive shaft, an annular solid = two turns: the same: and the entire rotating disk about the axis of the drive shaft and between the solid plate and the (four) disk The smashing space formed in the gap. 2 For example, the method of the third paragraph of the patent scope, wherein the organic porphyrin pigment, the perylene pigment, the Zhuang Yigong eucalyptus sulphur blue pigment, the second material is called the bismuth pigment, and the quinone pigment. ~4, ^_pigment, (4) pigment or dispersion 5.-type color for color 遽^, resin, its precursor or a mixture thereof;,:: transparent inclusion with a continuous kneading machine kneading package = and color ^ Wherein the mixture of the pigment-soluble organic liquid, the second; ', the water-based inorganic salt and the water-derived fine organic pigment, the continuous pinch 312 ΧΡ / invention specification (supplement) / 95·08/95114255 85 200706604 ;: Axis! Shaped fixed disk, concentric with the fixed disk and the entire formation of the powder ^ empty ^ turntable and in the gap between the fixed disk and the rotating disk, each! The colored composition of the fifth item of Legan Wai's in the mixture of the machine salt and 0.11 to, " ° parts by weight of the water-soluble organic liquid without I 。. Pigment "id" The coloring composition of the fifth item, wherein the machine-organic liquid-containing system is in the 10 cover, and the second color of the patent item 5, wherein the organic fat: water ☆ hot machine salt The mixture with the water-soluble organic liquid further comprises a coloring composition according to the fifth aspect of the patent application, wherein the mixture containing the machine >, hydrazine, watery inorganic salt and water-soluble organic liquid is more a derivative. — 10· A color filter comprising a color filter segment formed by the colored composition of claim 5, 312XP/invention specification (supplement)/95-08/95114255 86
TW095114255A 2005-04-22 2006-04-21 Process for the production of pigment composition, colored composition for color filter obtained by said process, and color filter TWI462975B (en)

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