WO2013129554A1 - Carbon black for black matrixes and method for producing same - Google Patents

Carbon black for black matrixes and method for producing same Download PDF

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Publication number
WO2013129554A1
WO2013129554A1 PCT/JP2013/055353 JP2013055353W WO2013129554A1 WO 2013129554 A1 WO2013129554 A1 WO 2013129554A1 JP 2013055353 W JP2013055353 W JP 2013055353W WO 2013129554 A1 WO2013129554 A1 WO 2013129554A1
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Prior art keywords
dye
carbon black
group
black
black matrix
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PCT/JP2013/055353
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French (fr)
Japanese (ja)
Inventor
浩幸 井戸川
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大同化成工業株式会社
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Application filed by 大同化成工業株式会社 filed Critical 大同化成工業株式会社
Priority to KR1020147027422A priority Critical patent/KR102027356B1/en
Priority to JP2014502355A priority patent/JP6425343B2/en
Priority to CN201380022565.3A priority patent/CN104245855B/en
Publication of WO2013129554A1 publication Critical patent/WO2013129554A1/en

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/56—Treatment of carbon black ; Purification
    • C09C1/565—Treatment of carbon black ; Purification comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/19—Oil-absorption capacity, e.g. DBP values
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/20—Filters
    • G02B5/22—Absorbing filters
    • G02B5/223—Absorbing filters containing organic substances, e.g. dyes, inks or pigments

Definitions

  • the present invention relates to carbon black for black matrix. Specifically, the present invention relates to carbon black for black matrix having high insulation and excellent concealment.
  • a metal thin film such as Cr is formed on a glass substrate by sputtering or the like, a photoresist is applied on the metal thin film, and ultraviolet light is irradiated through a photomask, followed by development processing.
  • a method of obtaining a resist pattern and removing unnecessary portions by etching or the like has been performed, but there is a problem that a metal abatement equipment is required and the manufacturing cost is high.
  • a method of forming a black matrix using a black matrix forming material in which carbon black is dispersed in a photopolymerizable compound is known. According to such a method, the black matrix can be manufactured at a very low cost because the material is inexpensive and the manufacturing process is simple. However, since carbon black has electrical conductivity, When the carbon black concentration is increased, the formed black matrix itself has conductivity, and there is a problem that it is easy to cause an image defect due to conduction between the transparent electrode on the color filter and the black matrix or between the counter electrodes. .
  • carbon black for black matrix has been proposed in which insulation is improved by coating carbon black with various resins (see, for example, Patent Documents 1 to 4). According to these methods, by forming a resin coating film on the surface of carbon black, ionic substances such as Ca and Na are contained, the contact between conductors is insulated, and further, jumping of electrons is impossible. Therefore, high insulation is achieved.
  • the above prior art has a problem that the ratio of carbon black in the black matrix is reduced by the amount of the coated resin, so that the concealability (OD) is lowered, and the contrast and color purity are lowered.
  • the manufacturing cost increases because the coating film of the black matrix has to be thickened.
  • organic solvents are used for the resin coating, it is necessary to take measures against safety during production and impact on the environment. For example, large-scale equipment such as workplace exhaust equipment, dryer explosion-proof equipment, wastewater treatment equipment, etc. There was a problem of requiring capital investment.
  • the present invention has been made in view of the above-described problems of the prior art, and the object of the present invention is to exhibit excellent concealability while maintaining high insulation in a color filter such as a liquid crystal display device, and is thin.
  • An object of the present invention is to provide a carbon black for a black matrix that can achieve high contrast and color purity even in a coating film.
  • Another object of the present invention is to provide a carbon black for a black matrix that can be manufactured safely and at low cost without adversely affecting the environment.
  • the present invention is carbon black for a black matrix in which the surface of carbon black is coated with a dye.
  • the present invention is also the carbon black for a black matrix according to (1), wherein the content of the dye is 0.5 to 10% by weight.
  • the present invention is also the carbon black for a black matrix according to (1) or (2), wherein the dye is an anionic or nonionic dye.
  • the present invention is also the carbon black for a black matrix according to any one of (1) to (3), wherein the dye is a dark color dye.
  • the present invention is also the carbon black for a black matrix according to any one of (1) to (4), wherein the dye is raked with a metal or a metal salt.
  • the present invention is also the carbon black for a black matrix according to (5), wherein the metal or metal salt is aluminum, magnesium, calcium, strontium, barium, manganese, or a salt thereof.
  • the present invention is also the carbon black for a black matrix according to any one of (1) to (6), wherein the carbon black has at least one acidic functional group on a surface.
  • the acidic functional group may be a hydroxyl group, oxo group, hydroperoxy group, carbonyl group, carboxyl group, peroxycarboxylic acid group, aldehyde group, ketone group, nitro group, nitroso group, amide group, imide.
  • the carbon black for a black matrix according to (7) which is a group, a sulfonic acid group, a sulfinic acid group, a sulfenic acid group, a thiocarboxylic acid group, a chlorosyl group, a chloryl group, a perchloryl group, an iodosyl group or an iodyl group.
  • the present invention is a method for producing carbon black for a black matrix, comprising a dye coating step of adding a dye to a carbon black slurry and coating the surface of the carbon black with a dye.
  • the present invention is also characterized in that, in the dye coating step, the dye is added so that the content of the dye in the resulting dye-coated carbon black is 0.5 to 10% by weight. It is a manufacturing method of carbon black for black matrices given in (9).
  • the present invention is also the method for producing carbon black for a black matrix according to (9) or (10), wherein the dye is an anionic or nonionic dye.
  • the present invention is also the method for producing carbon black for a black matrix according to any one of (9) to (11), wherein the dye is a dark color dye.
  • the present invention further includes a dye lake forming step in which the dye on the surface of the dye-coated carbon black obtained in the dye coating step is laked with a metal or a metal salt. It is a manufacturing method of carbon black for black matrices as described in one.
  • the present invention is also the method for producing carbon black for a black matrix according to (13), wherein the metal or metal salt is aluminum, magnesium, calcium, strontium, barium, manganese, or a salt thereof.
  • the oxidizing agent may be ozone gas, nitric acid, sodium hypochlorite, hydrogen peroxide, nitrogen monoxide gas, nitrogen dioxide gas, anhydrous sulfuric acid, fluorine gas, concentrated sulfuric acid, nitric acid, or various peroxides.
  • the carbon black for the black matrix of the present invention is formed by coating the surface of the carbon black with a dye, so that when used in a black matrix of a color filter such as a liquid crystal display device, it exhibits excellent concealment while maintaining high insulation.
  • a color filter such as a liquid crystal display device
  • high contrast and color purity can be achieved even with a thin coating film.
  • unlike conventional resin-coated carbon black it is not necessary to increase the thickness of the coating film in order to improve the concealing property, so that the manufacturing cost can be suppressed.
  • the carbon black for black matrix of the present invention is characterized in that the surface of carbon black is coated with a dye.
  • the type of raw material carbon black used in the present invention is not particularly limited, and known carbon blacks such as lamp black, acetylene black, thermal black, channel black, furnace black and the like can be used.
  • the raw material carbon black preferably has an average primary particle size of 5 to 60 nm, more preferably 10 to 50 nm, and particularly preferably 20 to 45 nm.
  • the average primary particle diameter means an arithmetic average value of particle diameters obtained by observing 1500 carbon black particles with an electron microscope. If the average primary particle size of the raw material carbon black is less than the above lower limit, aggregation tends to occur and the stability of the mill base is deteriorated and dispersion at a high concentration becomes difficult.On the other hand, if the upper limit is exceeded, the black matrix tends to cause shape defects. Since the surface roughness becomes worse, neither is preferable.
  • the raw material carbon black preferably has a DBP oil absorption of 100 ml / 100 g or less.
  • DBP oil absorption refers to the capacity of dibutyl phthalate (DBP) absorbed by 100 g of carbon black (JIS 6217).
  • DBP oil absorption amount of the raw material carbon black exceeds the above upper limit, the resistance value is decreased, and the viscosity is increased, so that the coating property is deteriorated and the blackness is decreased.
  • the raw material carbon black preferably has a pH value of 2 to 10, more preferably 5 to 9, and particularly preferably 4 to 8.
  • the pH value is a value obtained by measuring a mixed solution of carbon black and distilled water with a glass electrode pH meter (JIS 6221). If the pH of the raw material carbon black is less than the above lower limit, the overall balance is lost and the stability is deteriorated, and if it exceeds the upper limit, film peeling tends to occur.
  • the raw material carbon black those having an ash content of 1.0% or less and a specific surface area of 20 to 300 m 2 / g are preferably used. If the ash content exceeds the above upper limit, the resistance value decreases, which is not preferable, and if the specific surface area is less than the above lower limit, a black matrix shape is liable to occur, and if the upper limit is exceeded, a dispersant, resin, dye, etc. Since a large amount is required, neither is preferable.
  • the raw material carbon black is preferably oxidized in advance and has at least one acidic functional group on the surface, and two or more types of acidic functional groups are applied on the surface after a plurality of types of oxidation treatment. It is more preferable to have a group. Those that have not been oxidized in advance do not have acidic functional groups on the surface or the number of acidic functional groups is insufficient, so the dispersibility of the resulting carbon black for the black matrix cannot be ensured sufficiently, and the resistance value This is not preferable because the black matrix becomes insufficient and the insulating property of the black matrix becomes insufficient, and conduction between the transparent electrode on the color filter and the black matrix or between the counter electrodes tends to cause image defects.
  • Examples of such oxidation treatment include methods using ozone gas, nitric acid, sodium hypochlorite, hydrogen peroxide, nitrogen monoxide gas, nitrogen dioxide gas, sulfuric anhydride, fluorine gas, concentrated sulfuric acid, nitric acid, various peroxides, and the like.
  • the acidic functional group include a hydroxyl group, an oxo group, a hydroperoxy group, a carbonyl group, a carboxyl group, a peroxycarboxylic acid group, an aldehyde group, a ketone group, a nitro group, a nitroso group, an amide group, an imide group, and a sulfonic acid group.
  • the dye used in the present invention is not particularly limited as long as it can be adsorbed on the surface of carbon black, and a known basic dye, acid dye, direct dye, reactive dye, or the like is used.
  • anionic or non-ionic because the sulfone group or carboxyl group interacts with the functional group on the carbon black, the amino group reacts with the alkali-soluble resin, and it can be insolubilized with a sulfuric acid band, etc. Can be used more suitably.
  • a dark-colored dye having a high light absorption property close to black. Specific examples of such dyes include food color dyes such as Food Black No. 1, Food Black No.
  • Drimarene Brilliant Red X-2B Reactive Red 56
  • Levafix Brilliant Red E-4B Levafix Brilliant Red F-6BA
  • similar Reactive dyes such as Levafix® dyes Dystar (L. P.
  • the content of the dye in the carbon black for black matrix of the present invention is preferably 0.5 to 10% by mass, more preferably 1 to 7% by mass, and particularly preferably 1 to 5% by mass. If the content of the dye is less than the above lower limit, the coating is insufficient and a high resistance value cannot be obtained, and if the upper limit is exceeded, excess dye that is not coated tends to inhibit dispersibility and cause thickening and aggregation. Neither is preferred.
  • the dye is raked with a metal or a metal salt.
  • the dye is fixed to the surface of the carbon black or the acidic functional group via a metal or metal salt, and the dye is difficult to be detached from the surface of the carbon black, so that the dye is difficult to elute and has high shielding properties. Can be maintained.
  • the metal or metal salt used for rake formation include aluminum, magnesium, calcium, strontium, barium or manganese, and hydrochlorides, sulfates, and the like thereof. These may be used alone or in combination of two or more. be able to.
  • the addition amount of the metal or metal salt used for rake formation is preferably 0.3 times mol or more, more preferably 0.5 times mol or more, and particularly preferably 0.8 times mol or more with respect to the dye. If the addition amount of the metal or metal salt is less than the above, the dye is not sufficiently fixed, and it is easy to detach from the surface of the carbon black, and the stability of the mill base is poor and the resistance value is also not preferable.
  • carbon black as a raw material is mixed with water (prepared by appropriately mixing ion-exchanged water with tap water so that the electric conductivity is constant, the same shall apply hereinafter) to form a slurry, which is heated and stirred for a predetermined time to obtain carbon black. After washing, cool and wash again with water.
  • water is added to the obtained carbon black to form a slurry again, and the above-described oxidizing agent is added and stirred at a predetermined temperature for a predetermined time to oxidize the surface of the carbon black and rinse with water.
  • the oxidation treatment is carried out by changing the type of the oxidizing agent a plurality of times as necessary.
  • the obtained oxidized carbon black was mixed with water to form a slurry again, and a dye was added so as to have the predetermined content with respect to the target black matrix carbon black.
  • a dye was added so as to have the predetermined content with respect to the target black matrix carbon black.
  • equimolar amount of the above-mentioned metal or metal salt is added to the added dye and stirred at 30 to 70 ° C. for 1 to 5 hours to rake the dye with the metal or metal salt to fix the dye on the surface of carbon black. Let Then, this is cooled, washed with water, and filtered and dried to obtain the target carbon black for black matrix.
  • the carbon black for black matrix of the present invention can be mixed and dispersed with a photocurable resin or a photopolymerizable compound and a solvent and used as a composition for forming a black matrix.
  • the photopolymerizable compound is not particularly limited as long as it is cured to form a film when irradiated with ultraviolet rays, and a known photopolymerizable compound can be used. Specifically, acrylic acid, methacrylic acid, maleic acid, maleimide, crotonic acid, itaconic acid, cinnamic acid, vinyl alcohol, etc. and their derivatives; reaction with these and compounds having isocyanate groups, acid anhydride groups, etc.
  • alkali-soluble functional group such as a carboxyl group or a phenolic hydroxyl group in the structure and having alkali developability are preferred, and those having a bisphenolfluorene type epoxy diacrylate structure are particularly preferred.
  • the solvent examples include propylene glycol monomethyl ether acetate, methoxybutyl acetate cyclohexanone, ethyl cellosolve acetate, butyl cellosolve acetate, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, ethylene glycol diethyl ether, xylene, ethyl cellosolve, methyl-n amyl ketone, propylene glycol monomethyl ether , Toluene, methyl ethyl ketone, ethyl acetate, methanol, ethanol, isopropyl alcohol, butanol, isobutyl ketone, and the like.
  • Propylene glycol monomethyl ether acetate methoxybutyl acetate, cyclohexanone, and the like are particularly preferably used.
  • 10 g of slurry was prepared by mixing 1000 g of carbon black (TPX-1099: manufactured by cabot) with water, stirred at 95 ° C. for 1 hour, allowed to cool, and then washed with water. This was again mixed with water to prepare 10 L of slurry, 42.9 g of 70% nitric acid was added, and the mixture was stirred at 40 ° C. for 4 hours. This was allowed to cool and washed with water, and then mixed with water again to prepare 10 L of slurry, and 769.2 g of 13% sodium hypochlorite aqueous solution was added and stirred at 40 ° C. for 6 hours.
  • carbon black TPX-1099: manufactured by cabot
  • the acidic functional group amount (carboxyl group amount) of the obtained dye-coated carbon black was measured as follows according to the method described in JP-A-2000-248197.
  • Carboxyl group amount (50/20 ⁇ 0.01 ⁇ (titrated amount ⁇ empty titrated amount)) / carbon black sample mass
  • the amount of carboxyl groups of the obtained dye-coated carbon black was 53.9 mmol / g.
  • a carbon black for a black matrix according to the present invention was obtained in the same manner as in Example 1 except that the oxidation treatment with nitric acid and an aqueous sodium hypochlorite solution was not performed.
  • the amount of carboxyl groups in the obtained dye-coated carbon black was 3.4 mmol / g.
  • a comparative black matrix carbon black was obtained in the same manner as in Example 1 except that the dye coating and the rake treatment with aluminum sulfate were not performed.
  • Cyclohexanone was added to polyvinyl chloride (Nissan Vinyl E-430, manufactured by Nissan Chemical Co., Ltd.) and heated to about 90 ° C. to dissolve, thereby preparing a cyclohexanone solution containing 10% by weight of polyvinyl chloride.
  • carbon black furnace black, manufactured by Mitsubishi Chemical Corporation # 3050, average primary particle size 0.04 ⁇ m, specific surface area 50 m 2 / g (BET method)
  • water are mixed and stirred vigorously to obtain carbon black.
  • a uniform suspension containing 6 wt% was prepared. Next, the suspension was added to the cyclohexanone solution with stirring, and the carbon black in the aqueous phase was transferred to the solvent phase.
  • the water separated from the carbon black was removed by decantation, and then kneaded for about 5 minutes with a roll mill having two rolls heated to 80 to 120 ° C. to obtain a resin composition.
  • the resin composition is cut into a sheet shape with a heated roll, passed through a roll mill having two rolls at room temperature, pulverized to a size of about 30 mm or less, transferred to water, and at a speed of about 3000 rpm.
  • the mixture was agitated for about 3 minutes and pulverized and sized so as to be a granular material having a particle size of 0.1 to 3 mm, thereby obtaining a sized product.
  • the sized product was dried at 80 to 150 ° C. to obtain carbon black coated with a resin. [Evaluation]
  • the coating solution obtained above was applied to a glass substrate with a spin coater, dried at 90 ° C. for 2 minutes, and further heated and cured at 220 ° C. for 30 minutes to obtain a dried coating film.
  • the OD value of the obtained dried coating film was measured using a reflection densitometer, the film thickness and surface roughness were measured using Tencor Alpha Step IQ, and the surface resistance was measured using a surface resistance measuring instrument ("HIRESTA” manufactured by Dia Instruments Co., Ltd.). The results are shown in Table 1.
  • the carbon black for black matrix of the present invention (Examples 1 and 2) has an extremely high surface resistance as compared with the carbon black without dye coating (Comparative Example 1). It was found that an extremely high OD value was obtained as compared with the resin-coated carbon black (Comparative Example 2).
  • the carbon black for black matrix of the present invention has high insulating properties and excellent concealing properties, it is extremely useful when used for a black matrix of a color filter such as a liquid crystal display device.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Optical Filters (AREA)

Abstract

Provided is a carbon black for black matrixes, which has high insulation properties and excellent concealability. A carbon black for black matrixes, the surface of which is coated with an anionic or nonionic dark color dye. The carbon black has at least one kind of acidic functional group on the surface, and the dye is laked by a metal and affixed to the surface of the carbon black or to the acidic functional group.

Description

ブラックマトリックス用カーボンブラック及びその製造方法Carbon black for black matrix and method for producing the same
　本発明はブラックマトリックス用カーボンブラックに関する。詳しくは、高い絶縁性と優れた隠蔽性を備えたブラックマトリックス用カーボンブラックに関するものである。 The present invention relates to carbon black for black matrix. Specifically, the present invention relates to carbon black for black matrix having high insulation and excellent concealment.
　液晶表示装置等に使用されるカラーフィルターでは、異なる色相に着色された画素間にブラックマトリックスを形成することにより、光を遮断してコントラストを向上させ色純度の低下を防止している。 In color filters used in liquid crystal display devices and the like, by forming a black matrix between pixels colored in different hues, light is blocked to improve contrast and prevent a decrease in color purity.
　かかるブラックマトリックスの形成方法としては、従来、ガラス基板上にスパッタ等によりＣｒ等の金属薄膜を形成し、この金属薄膜上にフォトレジストを塗布してフォトマスクを介して紫外線を照射した後現像処理してレジストパターンを得、エッチング等により不要部分を除去する方法が行われていたが、金属除害設備等が必要であり製造コストも高いという問題があった。 As a method for forming such a black matrix, conventionally, a metal thin film such as Cr is formed on a glass substrate by sputtering or the like, a photoresist is applied on the metal thin film, and ultraviolet light is irradiated through a photomask, followed by development processing. Thus, a method of obtaining a resist pattern and removing unnecessary portions by etching or the like has been performed, but there is a problem that a metal abatement equipment is required and the manufacturing cost is high.
　これに対して、光重合性化合物にカーボンブラックを分散したブラックマトリックス形成材料を用いてブラックマトリックスを形成する方法が知られている。かかる方法によれば、材料が安価であり製造工程も簡略であるため極めて低コストでブラックマトリックスを製造することができるが、カーボンブラックは導電性を有するため、遮光性を上げるために樹脂中のカーボンブラック濃度を高くすると形成されたブラックマトリックス自体も導電性を有してしまい、カラーフィルター上の透明電極とブラックマトリックスの間や対向電極間で導通して画像不良を引き起こし易いという問題があった。 On the other hand, a method of forming a black matrix using a black matrix forming material in which carbon black is dispersed in a photopolymerizable compound is known. According to such a method, the black matrix can be manufactured at a very low cost because the material is inexpensive and the manufacturing process is simple. However, since carbon black has electrical conductivity, When the carbon black concentration is increased, the formed black matrix itself has conductivity, and there is a problem that it is easy to cause an image defect due to conduction between the transparent electrode on the color filter and the black matrix or between the counter electrodes. .
　そこで、カーボンブラックを種々の樹脂で被覆することにより絶縁性を改善したブラックマトリックス用カーボンブラックが提案されている（例えば、特許文献１～４参照）。これらの方法によれば、カーボンブラックの表面に樹脂被覆膜が形成されることにより、ＣａやＮａ等のイオン性物質が封じ込められ、導体同士の接触が絶縁され、更には電子のジャンプが不能になるため、高絶縁性が達成されるものである。 Therefore, carbon black for black matrix has been proposed in which insulation is improved by coating carbon black with various resins (see, for example, Patent Documents 1 to 4). According to these methods, by forming a resin coating film on the surface of carbon black, ionic substances such as Ca and Na are contained, the contact between conductors is insulated, and further, jumping of electrons is impossible. Therefore, high insulation is achieved.
特開平９－１２４９６９号公報JP-A-9-124969 特開平１１－０８０５８４号公報JP-A-11-080584 特開２００１－１５２０４６号公報JP 2001-152046 A 特開２００２－２４９６７８号公報JP 2002-249678 A
　しかしながら、上記従来技術では、被覆された樹脂の分だけブラックマトリックス中のカーボンブラックの比率が低下するため隠蔽性（ＯＤ）が低くなり、コントラストや色純度が低下してしまうという問題があり、そのために、ブラックマトリックスの塗膜を厚くしなければならなくなって、製造コストが増大するという問題があった。また、樹脂被覆に有機溶剤を使用するため製造時の安全性や環境への影響等についての対策が必要であり、例えば作業場の排気設備や乾燥機の防爆設備、廃水の処理設備等の大掛かりな設備投資が必要になるという問題があった。 However, the above prior art has a problem that the ratio of carbon black in the black matrix is reduced by the amount of the coated resin, so that the concealability (OD) is lowered, and the contrast and color purity are lowered. In addition, there is a problem that the manufacturing cost increases because the coating film of the black matrix has to be thickened. In addition, since organic solvents are used for the resin coating, it is necessary to take measures against safety during production and impact on the environment. For example, large-scale equipment such as workplace exhaust equipment, dryer explosion-proof equipment, wastewater treatment equipment, etc. There was a problem of requiring capital investment.
　本発明は上記従来技術の有する問題点に鑑みなされたものであり、その目的とするところは、液晶表示装置等のカラーフィルターにおいて、高い絶縁性を保持しつつ優れた隠蔽性を発揮し、薄い塗膜でも高いコントラストや色純度を達成することができるブラックマトリックス用カーボンブラックを提供することにある。 The present invention has been made in view of the above-described problems of the prior art, and the object of the present invention is to exhibit excellent concealability while maintaining high insulation in a color filter such as a liquid crystal display device, and is thin. An object of the present invention is to provide a carbon black for a black matrix that can achieve high contrast and color purity even in a coating film.
　本発明の他の目的は、環境に悪影響を与えず安全かつ低コストに製造することができるブラックマトリックス用カーボンブラックを提供することにある。 Another object of the present invention is to provide a carbon black for a black matrix that can be manufactured safely and at low cost without adversely affecting the environment.
　本発明の上記目的は、下記の手段によって達成される。 The above object of the present invention is achieved by the following means.
　（１）すなわち、本発明は、カーボンブラックの表面が染料で被覆されてなる、ブラックマトリックス用カーボンブラックである。 (1) That is, the present invention is carbon black for a black matrix in which the surface of carbon black is coated with a dye.
　（２）本発明はまた、前記染料の含有率が、０．５～１０重量％である、（１）に記載のブラックマトリックス用カーボンブラックである。 (2) The present invention is also the carbon black for a black matrix according to (1), wherein the content of the dye is 0.5 to 10% by weight.
　（３）本発明はまた、前記染料は、陰イオン性又は非イオン性の染料である、（１）又は（２）に記載のブラックマトリックス用カーボンブラックである。 (3) The present invention is also the carbon black for a black matrix according to (1) or (2), wherein the dye is an anionic or nonionic dye.
　（４）本発明はまた、前記染料は、濃色系の染料である、（１）乃至（３）の何れか１つに記載のブラックマトリックス用カーボンブラックである。 (4) The present invention is also the carbon black for a black matrix according to any one of (1) to (3), wherein the dye is a dark color dye.
　（５）本発明はまた、前記染料は、金属又は金属塩によりレーキ化されている、（１）乃至（４）の何れか１つに記載のブラックマトリックス用カーボンブラックである。 (5) The present invention is also the carbon black for a black matrix according to any one of (1) to (4), wherein the dye is raked with a metal or a metal salt.
　（６）本発明はまた、前記金属又は金属塩は、アルミニウム、マグネシウム、カルシウム、ストロンチウム、バリウム若しくはマンガン又はこれらの塩である、（５）に記載のブラックマトリックス用カーボンブラックである。 (6) The present invention is also the carbon black for a black matrix according to (5), wherein the metal or metal salt is aluminum, magnesium, calcium, strontium, barium, manganese, or a salt thereof.
　（７）本発明はまた、前記カーボンブラックは、表面に少なくとも１種類の酸性官能基を有する、（１）乃至（６）の何れか１つに記載のブラックマトリックス用カーボンブラックである。 (7) The present invention is also the carbon black for a black matrix according to any one of (1) to (6), wherein the carbon black has at least one acidic functional group on a surface.
　（８）本発明はまた、前記酸性官能基は、水酸基、オキソ基、ヒドロペルオキシ基、カルボニル基、カルボキシル基、ペルオキシカルボン酸基、アルデヒド基、ケトン基、ニトロ基、ニトロソ基、アミド基、イミド基、スルホン酸基、スルフィン酸基、スルフェン酸基、チオカルボン酸基、クロロシル基、クロリル基、ペルクロリル基、ヨードシル基又はヨージル基である、（７）に記載のブラックマトリックス用カーボンブラックである。 (8) In the present invention, the acidic functional group may be a hydroxyl group, oxo group, hydroperoxy group, carbonyl group, carboxyl group, peroxycarboxylic acid group, aldehyde group, ketone group, nitro group, nitroso group, amide group, imide. The carbon black for a black matrix according to (7), which is a group, a sulfonic acid group, a sulfinic acid group, a sulfenic acid group, a thiocarboxylic acid group, a chlorosyl group, a chloryl group, a perchloryl group, an iodosyl group or an iodyl group.
　（９）更に、本発明は、カーボンブラックのスラリーに染料を添加して、カーボンブラックの表面を染料で被覆する染料被覆工程を有する、ブラックマトリックス用カーボンブラックの製造方法である。 (9) Furthermore, the present invention is a method for producing carbon black for a black matrix, comprising a dye coating step of adding a dye to a carbon black slurry and coating the surface of the carbon black with a dye.
　（１０）本発明はまた、前記染料被覆工程は、得られる染料被覆カーボンブラック中の前記染料の含有率が０．５～１０重量％となるように前記染料を添加することを特徴とする、（９）に記載のブラックマトリックス用カーボンブラックの製造方法である。 (10) The present invention is also characterized in that, in the dye coating step, the dye is added so that the content of the dye in the resulting dye-coated carbon black is 0.5 to 10% by weight. It is a manufacturing method of carbon black for black matrices given in (9).
　（１１）本発明はまた、前記染料は、陰イオン性又は非イオン性の染料である、（９）又は（１０）に記載のブラックマトリックス用カーボンブラックの製造方法である。 (11) The present invention is also the method for producing carbon black for a black matrix according to (9) or (10), wherein the dye is an anionic or nonionic dye.
　（１２）本発明はまた、前記染料は、濃色系の染料である、（９）乃至（１１）の何れか１つに記載のブラックマトリックス用カーボンブラックの製造方法である。 (12) The present invention is also the method for producing carbon black for a black matrix according to any one of (9) to (11), wherein the dye is a dark color dye.
　（１３）本発明はまた、前記染料被覆工程で得られた染料被覆カーボンブラック表面の染料を金属又は金属塩によりレーキ化する染料レーキ化工程を更に有する、（９）乃至（１２）の何れか１つに記載のブラックマトリックス用カーボンブラックの製造方法である。 (13) The present invention further includes a dye lake forming step in which the dye on the surface of the dye-coated carbon black obtained in the dye coating step is laked with a metal or a metal salt. It is a manufacturing method of carbon black for black matrices as described in one.
　（１４）本発明はまた、前記金属又は金属塩は、アルミニウム、マグネシウム、カルシウム、ストロンチウム、バリウム若しくはマンガン又はこれらの塩である、（１３）に記載のブラックマトリックス用カーボンブラックの製造方法である。 (14) The present invention is also the method for producing carbon black for a black matrix according to (13), wherein the metal or metal salt is aluminum, magnesium, calcium, strontium, barium, manganese, or a salt thereof.
　（１５）本発明はまた、前記染料被覆工程に供する前記カーボンブラックの表面を酸化剤で酸化処理する酸化処理工程を更に有する、（９）乃至（１４）の何れか１つに記載のブラックマトリックス用カーボンブラックの製造方法である。 (15) The black matrix according to any one of (9) to (14), further comprising an oxidation treatment step of oxidizing the surface of the carbon black subjected to the dye coating step with an oxidizing agent. It is a manufacturing method of carbon black for use.
　（１６）本発明はまた、前記酸化剤は、オゾンガス、硝酸、次亜塩素酸ナトリウム、過酸化水素、一酸化窒素ガス、二酸化窒素ガス、無水硫酸、フッ素ガス、濃硫酸、硝酸又は各種過酸化物である、（１５）に記載のブラックマトリックス用カーボンブラックの製造方法である。 (16) In the present invention, the oxidizing agent may be ozone gas, nitric acid, sodium hypochlorite, hydrogen peroxide, nitrogen monoxide gas, nitrogen dioxide gas, anhydrous sulfuric acid, fluorine gas, concentrated sulfuric acid, nitric acid, or various peroxides. The method for producing carbon black for black matrix according to (15), which is a product.
　本発明のブラックマトリックス用カーボンブラックは、カーボンブラックの表面が染料で被覆されてなるので、液晶表示装置等のカラーフィルターのブラックマトリックスに用いた場合高い絶縁性を保持しつつ優れた隠蔽性を発揮し、薄い塗膜でも高いコントラストや色純度を達成することができる。また、従来の樹脂被覆カーボンブラックのように、隠蔽性を向上させるため塗膜を厚くする必要がないので、製造コストを抑えることができる。 The carbon black for the black matrix of the present invention is formed by coating the surface of the carbon black with a dye, so that when used in a black matrix of a color filter such as a liquid crystal display device, it exhibits excellent concealment while maintaining high insulation. However, high contrast and color purity can be achieved even with a thin coating film. Further, unlike conventional resin-coated carbon black, it is not necessary to increase the thickness of the coating film in order to improve the concealing property, so that the manufacturing cost can be suppressed.
　さらに、従来の樹脂被覆カーボンブラックのように有機溶剤を使用しないので、環境に悪影響等を与えることなく安全性に製造することができ、大掛かりな設備投資も必要としないので製造コストをより低減することができる。 Furthermore, unlike conventional resin-coated carbon black, no organic solvent is used, so it can be manufactured safely without adversely affecting the environment, and no significant capital investment is required, further reducing manufacturing costs. be able to.
　以下、本発明の実施の形態について詳細に説明する。 Hereinafter, embodiments of the present invention will be described in detail.
　本発明のブラックマトリックス用カーボンブラックは、カーボンブラックの表面が染料で被覆されてなることを特徴とするものである。 The carbon black for black matrix of the present invention is characterized in that the surface of carbon black is coated with a dye.
　本発明で利用される原料カーボンブラックの種類は特に限定されるものではなく、ランプブラック、アセチレンブラック、サーマルブラック、チャンネルブラック、ファーネスブラック等の既知のカーボンブラックを利用することができる。 The type of raw material carbon black used in the present invention is not particularly limited, and known carbon blacks such as lamp black, acetylene black, thermal black, channel black, furnace black and the like can be used.
　また、原料カーボンブラックは、平均一次粒子径が５～６０ｎｍのものが好ましく、１０～５０ｎｍのものがより好ましく、２０～４５ｎｍのものが特に好ましい。ここで、平均一次粒子径とは、カーボンブラック粒子１５００個を電子顕微鏡で観察して求めた粒子径の相加平均値をいう。原料カーボンブラックの平均一次粒子径が上記下限未満では、凝集を起こしやすくミルベースの安定性が悪くなり高濃度での分散が困難になる一方、上記上限を超えると、ブラックマトリックスが形状不良を生じやすくなり表面粗さも悪くなるので、何れも好ましくない。 The raw material carbon black preferably has an average primary particle size of 5 to 60 nm, more preferably 10 to 50 nm, and particularly preferably 20 to 45 nm. Here, the average primary particle diameter means an arithmetic average value of particle diameters obtained by observing 1500 carbon black particles with an electron microscope. If the average primary particle size of the raw material carbon black is less than the above lower limit, aggregation tends to occur and the stability of the mill base is deteriorated and dispersion at a high concentration becomes difficult.On the other hand, if the upper limit is exceeded, the black matrix tends to cause shape defects. Since the surface roughness becomes worse, neither is preferable.
　また、原料カーボンブラックは、ＤＢＰ吸油量が１００ｍｌ／１００ｇ以下のものが好ましい。ここで、ＤＢＰ吸油量とは、カーボンブラック１００ｇが吸収するフタル酸ジブチル（ＤＢＰ）の容量をいう（ＪＩＳ６２１７）。原料カーボンブラックのＤＢＰ吸油量が上記上限を超えると、抵抗値が低下し、また、粘度が高くなるので塗布性が悪くなり、黒色度が低下したりするので好ましくない。 The raw material carbon black preferably has a DBP oil absorption of 100 ml / 100 g or less. Here, DBP oil absorption refers to the capacity of dibutyl phthalate (DBP) absorbed by 100 g of carbon black (JIS 6217). When the DBP oil absorption amount of the raw material carbon black exceeds the above upper limit, the resistance value is decreased, and the viscosity is increased, so that the coating property is deteriorated and the blackness is decreased.
　さらに、原料カーボンブラックは、ｐＨ値が２～１０のものが好ましく、５～９のものがより好ましく、４～８のものが特に好ましい。ここで、ｐＨ値とは、カーボンブラックと蒸留水の混合液をガラス電極ｐＨ計で測定した値をいう（ＪＩＳ６２２１）。原料カーボンブラックのｐＨが上記下限未満では全体のバランスが崩れ安定性が悪くなり、上記上限を超えると膜剥がれが生じやすくなるので何れも好ましくない。 Furthermore, the raw material carbon black preferably has a pH value of 2 to 10, more preferably 5 to 9, and particularly preferably 4 to 8. Here, the pH value is a value obtained by measuring a mixed solution of carbon black and distilled water with a glass electrode pH meter (JIS 6221). If the pH of the raw material carbon black is less than the above lower limit, the overall balance is lost and the stability is deteriorated, and if it exceeds the upper limit, film peeling tends to occur.
　さらに、原料カーボンブラックは、灰分が１．０％以下、比表面積が２０～３００ｍ２／ｇのものが好適に利用される。灰分が上記上限を超えると抵抗値が低下するので好ましくなく、また、比表面積が、上記下限を下回るとブラックマトリックスの形状不良が生じやすくなり、上記上限を超えると分散剤、樹脂、染料等を多量に必要とするため、何れも好ましくない。 Further, as the raw material carbon black, those having an ash content of 1.0% or less and a specific surface area of 20 to 300 m 2 / g are preferably used. If the ash content exceeds the above upper limit, the resistance value decreases, which is not preferable, and if the specific surface area is less than the above lower limit, a black matrix shape is liable to occur, and if the upper limit is exceeded, a dispersant, resin, dye, etc. Since a large amount is required, neither is preferable.
　また、原料カーボンブラックは、事前に酸化処理が施されて表面に少なくとも１種類の酸性官能基を有していることが好ましく、複数種類の酸化処理が施されて表面に２種類以上の酸性官能基を有していることがより好ましい。事前に酸化処理が施されていないものは表面に酸性官能基を有しないか酸性官能基の数が不十分であるため、得られるブラックマトリックス用カーボンブラックの分散性が十分に確保できず抵抗値が低下してブラックマトリックスの絶縁性が不十分となり、カラーフィルター上の透明電極とブラックマトリックスの間や対向電極間で導通して画像不良を引き起こし易くなるので好ましくない。かかる酸化処理としては、オゾンガス、硝酸、次亜塩素酸ナトリウム、過酸化水素、一酸化窒素ガス、二酸化窒素ガス、無水硫酸、フッ素ガス、濃硫酸、硝酸、各種過酸化物等を用いる方法が挙げられ、前記酸性官能基としては、水酸基、オキソ基、ヒドロペルオキシ基、カルボニル基、カルボキシル基、ペルオキシカルボン酸基、アルデヒド基、ケトン基、ニトロ基、ニトロソ基、アミド基、イミド基、スルホン酸基、スルフィン酸基、スルフェン酸基、チオカルボン酸基、クロロシル基、クロリル基、ペルクロリル基、ヨードシル基、ヨージル基等が挙げられる。 The raw material carbon black is preferably oxidized in advance and has at least one acidic functional group on the surface, and two or more types of acidic functional groups are applied on the surface after a plurality of types of oxidation treatment. It is more preferable to have a group. Those that have not been oxidized in advance do not have acidic functional groups on the surface or the number of acidic functional groups is insufficient, so the dispersibility of the resulting carbon black for the black matrix cannot be ensured sufficiently, and the resistance value This is not preferable because the black matrix becomes insufficient and the insulating property of the black matrix becomes insufficient, and conduction between the transparent electrode on the color filter and the black matrix or between the counter electrodes tends to cause image defects. Examples of such oxidation treatment include methods using ozone gas, nitric acid, sodium hypochlorite, hydrogen peroxide, nitrogen monoxide gas, nitrogen dioxide gas, sulfuric anhydride, fluorine gas, concentrated sulfuric acid, nitric acid, various peroxides, and the like. Examples of the acidic functional group include a hydroxyl group, an oxo group, a hydroperoxy group, a carbonyl group, a carboxyl group, a peroxycarboxylic acid group, an aldehyde group, a ketone group, a nitro group, a nitroso group, an amide group, an imide group, and a sulfonic acid group. , Sulfinic acid group, sulfenic acid group, thiocarboxylic acid group, chlorosyl group, chloryl group, perchloryl group, iodosyl group, iodyl group and the like.
　本発明で利用される染料としては、カーボンブラックの表面に吸着可能なものであれば特に限定されるものではなく、既知の塩基性染料、酸性染料、直接染料、反応性染料等を利用することができるが、スルホン基やカルボキシル基がカーボンブラック上の官能基と相互作用すること、アミノ基とアルカリ可溶性樹脂が反応してしまうこと、硫酸バンド等で不溶化できること等から、陰イオン性又は非イオン性の染料がより好適に利用できる。また、得られるブラックマトリックスの遮光性をより高いものにするため光吸収性の高い黒色に近い濃色系の染料を用いることが好ましい。このような染料の具体例としては、Food Black No.1、Food Black No.2、Food Red No.40、Food Blue No.1、Food Yellow No.7等の食用色素染料、Bernacid Red 2BMN、Basacid Black X34(BASF X-34)（BASF社製）、Kayanol Red 3BL(Nippon Kayaku Company社製)、Dermacarbon 2GT(Sandoz社製)、Telon Fast Yellow 4GL-175、BASF Basacid Black SE 0228、Basacid Black X34(BASF X-34)（BASF社製）、Basacid Blue 750(BASF社製)、Bernacid Red（Bemcolors, Poughkeepsie, N. Y. 社製）、BASF Basacid Black SE 0228（BASF社製）等の各色の酸性染料、Pontamine Brilliant Bond Blue A及びその他のPontamine Brilliant Bond Blue A及びその他のPontamine（登録商標）染料（Bayer Chemicals Corporation、Pittsburgh,PA社製)、Cartasol Yellow GTF Presscake（Sandoz, Inc社製）;Cartasol Yellow GTF Liquid Special 110（Sandoz, Inc. 社製）;Yellow Shade 16948（Tricon社製）、Direct Brilliant Pink B(Crompton & Knowles社製)、Carta Black 2GT（Sandoz, Inc. 社製）、Sirius Supra Yellow GD 167、Cartasol Brilliant Yellow 4GF(Sandoz社製);、Pergasol Yellow CGP(Ciba-Geigy社製)、Pyrazol Black BG(JCI社製)、Diazol Black RN Quad(JCJ社製)、Pontamine Brilliant Bond Blue; Berncolor A. Y. 34等の各色の直接染料、Cibacron Brilliant Red 3B-A(Reactive Red 4)（Aldrich Chemical、Milwaukee, WI社製)、Drimarene Brilliant Red X-2B(Reactive Red 56)（Pylam Products, Inc. Tempe, AZ社製)、Levafix Brilliant Red E-4B,Levafix Brilliant Red F-6BA,及び類似のLevafix（登録商標）dyes Dystar L. P.(Charlotte, NC社製)製の染料、Procion Red H8B(Reactive Red 31)（JCI America社製）、等の各色の反応性染料、Neozapon Red 492(BASF社製)、Orasol Red G(Ciba-Geigy社製)、Aizen Spilon RedC-BH(Hodogaya Chemical Company社製)、Spirit Fast Yellow 3G、Aizen Spilon Yellow C-GNH(Hodogaya Chemical Company社製)、Orasol Black RL(Ciba-Geigy社製)、Orasol Black RLP(Ciba-Geigy社製)、Savinyl Black RLS(Sandoz社製)、Orasol Blue GN (Ciba-Geigy社製)、Luxol BlueMBSN (Morton-Thiokol社製)、Morfast Black Concentrate A(Morton-Thiokol社製)等の油溶性染料等が挙げられる。これらは単独で利用されてもよいし又は２種以上を組み合わせて利用されてもよい。 The dye used in the present invention is not particularly limited as long as it can be adsorbed on the surface of carbon black, and a known basic dye, acid dye, direct dye, reactive dye, or the like is used. However, anionic or non-ionic, because the sulfone group or carboxyl group interacts with the functional group on the carbon black, the amino group reacts with the alkali-soluble resin, and it can be insolubilized with a sulfuric acid band, etc. Can be used more suitably. Moreover, in order to make the black matrix obtained have a higher light-shielding property, it is preferable to use a dark-colored dye having a high light absorption property close to black. Specific examples of such dyes include food color dyes such as Food Black No. 1, Food Black No. 2, Food Red No. 40, Food Blue No. 1, Food Yellow Yellow No. 7, Bernacid Red Red 2BMN, Basacid Black X34 (BASF X-34) (BASF), Kayanol Red 3BL (Nippon Kayaku Company), Dermacarbon 2GT (Sandoz), Telon Fast Yellow 4GL-175, BASF Basacid Black SE 0228, Basacid Black X34 ( BASF X-34) (BASF), Basacid Blue 750 (BASF), Bernacid Red (Bemcolors, Poughkeepsie, N. Y.), BASF Basacid Black SE 0228 (BASF) Dye, Pontamine Brilliant Bond Blue A and other Pontamine Brilliant Bond Blue A and other Pontamine (R) dyes (Bayer Chemicals Corporation, Pittsburgh, PA), Cartasol Yellow GTF Presscake (Sandoz, Inc Y); Cartasol el GTF Liquid Special 110 (Sandoz, Inc.); Yellow Shade 16948 (Tricon), Direct Brilliant Pi nk B (Crompton & Knowles), Carta Black 2GT (Sandoz, Inc.), Sirius Supra Yellow GD 167, Cartasol Brilliant Yellow 4GF (Sandoz); Pergasol Yellow CGP (Ciba-Geigy) Pyrazol Black BG (manufactured by JCI), Diazol Black RN Quad (manufactured by JCJ), Pontamine Brilliant Bond Blue; Berncolor A. Y. 34, etc. Chemical, Milwaukee, WI), Drimarene Brilliant Red X-2B (Reactive Red 56) (Pylam Products, sInc. Tempe, AZ), Levafix Brilliant Red E-4B, Levafix Brilliant Red F-6BA, and similar Reactive dyes such as Levafix® dyes Dystar (L. P. (Charlotte, NC), Procion Red H8B (Reactive Red 31) (JCI America), Neozapon Red 492 (BASF Orasol Red G (Ciba-Geigy), Aizen Spilon RedC-BH (Hodogaya Chemical Company), Spirit Fast Yellow 3G, Aizen Spilon Yellow C-GNH (Hodogay a (Chemical Company), Orasol Black RL (Ciba-Geigy), Orasol Black RLP (Ciba-Geigy), Savinyl Black RLS (Sandoz), Orasol Blue GN (Ciba-Geigy), Luxol Examples include oil-soluble dyes such as BlueMBSN® (Morton-Thiokol), Morfast® Black® Concentrate® A (Morton-Thiokol). These may be used alone or in combination of two or more.
　また、本発明のブラックマトリックス用カーボンブラックにおける前記染料の含有量は、０．５～１０質量％が好ましく、１～７質量％がより好ましく、１～５質量％が特に好ましい。染料の含有量が上記下限未満では被覆が不十分となり高い抵抗値が得られず、上記上限を超えると被覆されなかった余剰の染料が分散性を阻害し増粘・凝集を起こし易くなるので、何れも好ましくない。 Further, the content of the dye in the carbon black for black matrix of the present invention is preferably 0.5 to 10% by mass, more preferably 1 to 7% by mass, and particularly preferably 1 to 5% by mass. If the content of the dye is less than the above lower limit, the coating is insufficient and a high resistance value cannot be obtained, and if the upper limit is exceeded, excess dye that is not coated tends to inhibit dispersibility and cause thickening and aggregation. Neither is preferred.
　さらに、本発明のブラックマトリックス用カーボンブラックは、金属又は金属塩により前記染料がレーキ化されていることが好ましい。かかるレーキ化により、染料が金属又は金属塩を介してカーボンブラックの表面や前記酸性官能基に固定され、染料がカーボンブラックの表面から離脱し難くなるので、染料が溶出し難くなり高い遮蔽性を維持することができる。かかるレーキ化に利用される金属又は金属塩としては、アルミニウム、マグネシウム、カルシウム、ストロンチウム、バリウム若しくはマンガン又はこれらの塩酸塩、硫酸塩等が挙げられ、これらを単独で又は２種以上を組み合わせて用いることができる。レーキ化に利用される金属又は金属塩の添加量は、染料に対して０．３倍モル以上が好ましく、０．５倍モル以上がより好ましく、０．８倍モル以上が特に好ましい。金属又は金属塩の添加量が上記未満では、染料の固定が不十分となりカーボンブラック表面から離脱し易くなり、ミルベースの安定性が悪く抵抗値も低下するので好ましくない。 Furthermore, in the carbon black for black matrix of the present invention, it is preferable that the dye is raked with a metal or a metal salt. By this rake formation, the dye is fixed to the surface of the carbon black or the acidic functional group via a metal or metal salt, and the dye is difficult to be detached from the surface of the carbon black, so that the dye is difficult to elute and has high shielding properties. Can be maintained. Examples of the metal or metal salt used for rake formation include aluminum, magnesium, calcium, strontium, barium or manganese, and hydrochlorides, sulfates, and the like thereof. These may be used alone or in combination of two or more. be able to. The addition amount of the metal or metal salt used for rake formation is preferably 0.3 times mol or more, more preferably 0.5 times mol or more, and particularly preferably 0.8 times mol or more with respect to the dye. If the addition amount of the metal or metal salt is less than the above, the dye is not sufficiently fixed, and it is easy to detach from the surface of the carbon black, and the stability of the mill base is poor and the resistance value is also not preferable.
　次に、本発明のブラックマトリックス用カーボンブラックの製造方法について説明する。まず、原料のカーボンブラックを水（電気伝導度が一定となるよう水道水にイオン交換水を適宜混合して調製したもの、以下同じ）と混合してスラリーとし、所定時間加熱撹拌してカーボンブラックを洗浄処理し、冷却後再度水洗する。次に、得られたカーボンブラックに水を加えて再びスラリーとし、上述した酸化剤を添加して所定温度で所定時間撹拌してカーボンブラックの表面を酸化処理し、水洗する。酸化処理は、必要により複数回、酸化剤の種類を変えて行う。次いで、得られた酸化処理済のカーボンブラックを水と混合して再びスラリーとし、目的のブラックマトリックス用カーボンブラックに対して前記所定含有量となるよう染料を添加し、４０～９０℃で１～５時間撹拌して、カーボンブラックの表面に染料を吸着して被覆させる。更に、添加した染料と等モルの上述した金属又は金属塩を添加し、３０～７０℃で１～５時間撹拌して、染料を金属又は金属塩でレーキ化してカーボンブラックの表面に染料を固定させる。そして、これを冷却後水洗し、ろ過乾燥することにより、目的のブラックマトリックス用カーボンブラックを得ることができる。 Next, a method for producing carbon black for black matrix according to the present invention will be described. First, carbon black as a raw material is mixed with water (prepared by appropriately mixing ion-exchanged water with tap water so that the electric conductivity is constant, the same shall apply hereinafter) to form a slurry, which is heated and stirred for a predetermined time to obtain carbon black. After washing, cool and wash again with water. Next, water is added to the obtained carbon black to form a slurry again, and the above-described oxidizing agent is added and stirred at a predetermined temperature for a predetermined time to oxidize the surface of the carbon black and rinse with water. The oxidation treatment is carried out by changing the type of the oxidizing agent a plurality of times as necessary. Next, the obtained oxidized carbon black was mixed with water to form a slurry again, and a dye was added so as to have the predetermined content with respect to the target black matrix carbon black. Stir for 5 hours to adsorb and coat the dye on the carbon black surface. Furthermore, equimolar amount of the above-mentioned metal or metal salt is added to the added dye and stirred at 30 to 70 ° C. for 1 to 5 hours to rake the dye with the metal or metal salt to fix the dye on the surface of carbon black. Let Then, this is cooled, washed with water, and filtered and dried to obtain the target carbon black for black matrix.
　本発明のブラックマトリックス用カーボンブラックは、光硬化性樹脂又は光重合性化合物及び溶媒と混合、分散させて、ブラックマトリックス形成用組成物として利用することができる。かかる光重合性化合物としては、紫外線を照射すると硬化して被膜を形成するものであれば特に限定されるものではなく、既知の光重合性化合物を利用することができる。具体的には、アクリル酸、メタクリル酸、マレイン酸、マレイミド、クロトン酸、イタコン酸、ケイヒ酸、ビニルアルコール等及びこれらの誘導体；これらとイソシアネート基、酸無水物基等を有する化合物との反応生成物；ビニル樹脂、ポリエステル樹脂、ポリアミド樹脂、ポリイミド樹脂、ポリウレタン樹脂、ポリエーテル樹脂等の主鎖又は側鎖にエステル結合、アミド結合、ウレタン結合等を介してアクリロイル基又はメタクリロイル基を導入した樹脂等が挙げられるが、構造中にカルボキシル基やフェノール性水酸基等のアルカリ溶解性官能基を有しアルカリ現像性を持つものが好ましく、特にビスフェノールフルオレン型エポキシジアクリレート構造を有するものが好ましい。また、前記溶媒としては、プロピレングリコールモノメチルエーテルアセテート、メトキシブチルアセテートシクロヘキサノン、エチルセロソルブアセテート、ブチルセロソルブアセテート、ジエチレングリコールジメチルエーテル、ジエチレングリコールジエチルエーテルエチレングリコールジエチルエーテル、キシレン、エチルセロソルブ、メチル－ｎアミルケトン、プロピレングリコールモノメチルエーテル、トルエン、メチルエチルケトン、酢酸エチル、メタノール、エタノール、イソプロピルアルコール、ブタノール、イソブチルケトン等が挙げられ、特にプロピレングリコールモノメチルエーテルアセテートメトキシブチルアセテート、シクロヘキサノン等が好適に利用される。 The carbon black for black matrix of the present invention can be mixed and dispersed with a photocurable resin or a photopolymerizable compound and a solvent and used as a composition for forming a black matrix. The photopolymerizable compound is not particularly limited as long as it is cured to form a film when irradiated with ultraviolet rays, and a known photopolymerizable compound can be used. Specifically, acrylic acid, methacrylic acid, maleic acid, maleimide, crotonic acid, itaconic acid, cinnamic acid, vinyl alcohol, etc. and their derivatives; reaction with these and compounds having isocyanate groups, acid anhydride groups, etc. Product: Resin having acryloyl group or methacryloyl group introduced into the main chain or side chain of vinyl resin, polyester resin, polyamide resin, polyurethane resin, polyether resin, etc. via ester bond, amide bond, urethane bond, etc. However, those having an alkali-soluble functional group such as a carboxyl group or a phenolic hydroxyl group in the structure and having alkali developability are preferred, and those having a bisphenolfluorene type epoxy diacrylate structure are particularly preferred. Examples of the solvent include propylene glycol monomethyl ether acetate, methoxybutyl acetate cyclohexanone, ethyl cellosolve acetate, butyl cellosolve acetate, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, ethylene glycol diethyl ether, xylene, ethyl cellosolve, methyl-n amyl ketone, propylene glycol monomethyl ether , Toluene, methyl ethyl ketone, ethyl acetate, methanol, ethanol, isopropyl alcohol, butanol, isobutyl ketone, and the like. Propylene glycol monomethyl ether acetate methoxybutyl acetate, cyclohexanone, and the like are particularly preferably used.
　次に、本発明のブラックマトリックス用カーボンブラックを実施例を示して更に詳細に説明するが、本発明はこれらの実施例に限定されるものではない。 Next, the carbon black for black matrix of the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
　染料被覆カーボンブラック（酸化処理あり）の調製 Preparation of dye-coated carbon black (with oxidation treatment)
　カーボンブラック（TPX-1099：cabot社製）１０００ｇを水と混合してスラリー１０Ｌを調製し、９５℃で１時間撹拌させ放冷した後水洗した。これを再び水と混合処理してスラリー１０Ｌを調製し、７０％の硝酸４２．９ｇを添加して４０℃で４時間撹拌した。これを放冷して水洗した後再び水と混合してスラリー１０Ｌを調製し、１３％の次亜塩素酸ナトリウム水溶液７６９．２ｇを添加して４０℃で６時間撹拌した。これを放冷して水洗した後再び水と混合してスラリー１０Ｌを調製し、純度３８．４％の染料（Direct Deep BLACK）３８．１ｇを添加して４０℃で１時間撹拌し、その後更に硫酸アルミニウム１０．１ｇを添加して４０℃で１時間撹拌した。これを放冷した後水洗し、ろ過乾燥させて、本発明のブラックマトリックス用カーボンブラックを得た。 10 g of slurry was prepared by mixing 1000 g of carbon black (TPX-1099: manufactured by cabot) with water, stirred at 95 ° C. for 1 hour, allowed to cool, and then washed with water. This was again mixed with water to prepare 10 L of slurry, 42.9 g of 70% nitric acid was added, and the mixture was stirred at 40 ° C. for 4 hours. This was allowed to cool and washed with water, and then mixed with water again to prepare 10 L of slurry, and 769.2 g of 13% sodium hypochlorite aqueous solution was added and stirred at 40 ° C. for 6 hours. This was allowed to cool, washed with water, mixed with water again to prepare 10 L of slurry, 38.1 g of a dye having a purity of 38.4% (Direct Deep BLACK) was added and stirred at 40 ° C. for 1 hour, and then further 10.1 g of aluminum sulfate was added and stirred at 40 ° C. for 1 hour. This was allowed to cool, washed with water, filtered and dried to obtain carbon black for black matrix of the present invention.
　カルボキシル基量の測定 Measurement of carboxyl group content
　得られた染料被覆カーボンブラックの酸性官能基量（カルボキシル基量）を、特開２０００－２４８１９７号公報に記載の方法に従って、以下のとおり測定した。 The acidic functional group amount (carboxyl group amount) of the obtained dye-coated carbon black was measured as follows according to the method described in JP-A-2000-248197.
　染料被覆カーボンブラック１０ｇを秤量し、０．１規定の炭酸水素ナトリウム水溶液５０ｍｌ中で１時間振盪して反応させた後濾過し、濾液の上澄み液２０ｍｌを採取して０．０１規定の塩酸水溶液で滴定した。カルボキシル基量は、カーボンブラック１ｇ中のミリモル量（ｍｍｏｌ／ｇ）として下式に従って求めた。 10 g of dye-coated carbon black was weighed, reacted by shaking in 50 ml of 0.1 N sodium bicarbonate aqueous solution for 1 hour, filtered, and 20 ml of the supernatant of the filtrate was collected and added with 0.01 N hydrochloric acid aqueous solution. Titration. The amount of carboxyl groups was determined according to the following formula as the amount of mmol (mmol / g) in 1 g of carbon black.
　カルボキシル基量＝（５０／２０×０．０１×（滴定量－空滴定量））／カーボンブラック試料質量 Carboxyl group amount = (50/20 × 0.01 × (titrated amount−empty titrated amount)) / carbon black sample mass
　得られた染料被覆カーボンブラックのカルボキシル基量は、５３．９ｍｍｏｌ／ｇであった。 The amount of carboxyl groups of the obtained dye-coated carbon black was 53.9 mmol / g.
　染料被覆カーボンブラック（酸化処理なし）の調製 Preparation of dye-coated carbon black (no oxidation treatment)
　硝酸及び次亜塩素酸ナトリウム水溶液による酸化処理を施さなかった以外は実施例１とほぼ同様に処理して、本発明のブラックマトリックス用カーボンブラックを得た。得られた染料被覆カーボンブラックのカルボキシル基量は、３．４ｍｍｏｌ／ｇであった。
［比較例１］ A carbon black for a black matrix according to the present invention was obtained in the same manner as in Example 1 except that the oxidation treatment with nitric acid and an aqueous sodium hypochlorite solution was not performed. The amount of carboxyl groups in the obtained dye-coated carbon black was 3.4 mmol / g.
[Comparative Example 1]
　染料未被覆カーボンブラックの調製 Preparation of dye-uncoated carbon black
　染料被覆及び硫酸アルミニウムによるレーキ処理を施さなかった以外は実施例１とほぼ同様に処理して、比較用のブラックマトリックス用カーボンブラックを得た。
［比較例２］ A comparative black matrix carbon black was obtained in the same manner as in Example 1 except that the dye coating and the rake treatment with aluminum sulfate were not performed.
[Comparative Example 2]
　樹脂被覆カーボンブラックの調製 Preparation of resin-coated carbon black
　ポリ塩化ビニル（日産化学（株）製ニッサンビニルＥ－４３０）にシクロヘキサノンを添加し、約９０℃に加熱して溶解させ、ポリ塩化ビニルを１０重量％含有したシクロヘキサノン溶液を調製した。一方、カーボンブラック（ファーネスブラック、三菱化学（株）製＃３０５０、平均一次粒子径０．０４μｍ、比表面積５０ｍ２／ｇ（ＢＥＴ法））と水とを混合して強力に撹拌し、カーボンブラックを６重量％含有した均一な懸濁液を調製した。次に、前記シクロヘキサノン溶液に懸濁液を撹拌しながら添加し、水相のカーボンブラックを溶剤相に移行させた。次いで、カーボンブラックと分離した水を、デカンテーションによって除去したのち、８０～１２０℃に加熱した２本のロールを有するロールミルで約５分間混練して樹脂組成物を得た。次に、樹脂組成物を加熱ロールによりシート状に切出し、これを常温の２本のロールを有するロールミルに通し、約３０ｍｍ以下の大きさにまで粉砕したのち、水中に移し、約３０００ｒｐｍの速度で約３分間撹拌して粒子径が０．１～３ｍｍの粒状物となるように粉砕整粒し、整粒物を得た。この整粒物を８０～１５０℃で乾燥し、樹脂で被覆されたカーボンブラックを得た。
［評価］ Cyclohexanone was added to polyvinyl chloride (Nissan Vinyl E-430, manufactured by Nissan Chemical Co., Ltd.) and heated to about 90 ° C. to dissolve, thereby preparing a cyclohexanone solution containing 10% by weight of polyvinyl chloride. On the other hand, carbon black (furnace black, manufactured by Mitsubishi Chemical Corporation # 3050, average primary particle size 0.04 μm, specific surface area 50 m 2 / g (BET method)) and water are mixed and stirred vigorously to obtain carbon black. A uniform suspension containing 6 wt% was prepared. Next, the suspension was added to the cyclohexanone solution with stirring, and the carbon black in the aqueous phase was transferred to the solvent phase. Next, the water separated from the carbon black was removed by decantation, and then kneaded for about 5 minutes with a roll mill having two rolls heated to 80 to 120 ° C. to obtain a resin composition. Next, the resin composition is cut into a sheet shape with a heated roll, passed through a roll mill having two rolls at room temperature, pulverized to a size of about 30 mm or less, transferred to water, and at a speed of about 3000 rpm. The mixture was agitated for about 3 minutes and pulverized and sized so as to be a granular material having a particle size of 0.1 to 3 mm, thereby obtaining a sized product. The sized product was dried at 80 to 150 ° C. to obtain carbon black coated with a resin.
[Evaluation]
　ブラックマトリックス用塗布液の調製 Preparation of coating liquid for black matrix
　実施例１及び２並びに比較例１及び２で得られたブラックマトリックス用カーボンブラックのそれぞれについて、ブラックマトリックス用カーボンブラック３００ｇと、ウレタン系分散剤のＢＹＫ－１６７（ビックケミー・ジャパン社製）４６．６ｇと、フルオレン骨格を有するエポキシアクリレート酸付加物のプロピレングリコールモノメチルエーテルアセテート溶液（樹脂固形分濃度＝５５．５質量％、新日鐵化学社製「Ｖ２５９ＭＥ」）１８９．２ｇとをビーズミルで分散してベースインクを得た。このベースインク２０ｇに、フルオレン骨格を有するエポキシアクリレート酸付加物のプロピレングリコールモノメチルエーテルアセテート溶液（樹脂固形分濃度＝５５．５質量％、新日鐵化学社製「Ｖ２５９ＭＥ」）３．５２ｇと、プロピレングリコールモノメチルエーテルアセテート２１．９ｇを添加して塗布液を調整した。 For each of the black black for black matrix obtained in Examples 1 and 2 and Comparative Examples 1 and 2, 300 g of black black for carbon black matrix and 46.6 g of urethane dispersant BYK-167 (by Big Chemie Japan) And 189.2 g of a propylene glycol monomethyl ether acetate solution of epoxy acrylate acid adduct having a fluorene skeleton (resin solid content concentration = 55.5% by mass, “V259ME” manufactured by Nippon Steel Chemical Co., Ltd.) was dispersed in a bead mill. A base ink was obtained. 20 g of this base ink, 3.52 g of a propylene glycol monomethyl ether acetate solution of an epoxy acrylate acid adduct having a fluorene skeleton (resin solid content concentration = 55.5% by mass, “V259ME” manufactured by Nippon Steel Chemical Co., Ltd.) and propylene A coating solution was prepared by adding 21.9 g of glycol monomethyl ether acetate.
　ＯＤ値、表面粗さ及び表面抵抗の測定 Measurement of OD value, surface roughness and surface resistance
　上記で得られた塗布液をガラス基板にスピンコーターで塗布し、９０℃で２分間乾燥し、更に２２０℃で３０分加熱して硬化させて乾燥塗膜を得た。 The coating solution obtained above was applied to a glass substrate with a spin coater, dried at 90 ° C. for 2 minutes, and further heated and cured at 220 ° C. for 30 minutes to obtain a dried coating film.
　得られた乾燥塗膜のＯＤ値を反射濃度計により、膜厚及び表面粗さをテンコール社アルファステップＩＱにより、表面抵抗を表面抵抗測定器（（株）ダイアインスツルメント社製「ハイレスタ」）により、それぞれ測定して、その結果を表１に示した。
Figure JPOXMLDOC01-appb-T000001
 The OD value of the obtained dried coating film was measured using a reflection densitometer, the film thickness and surface roughness were measured using Tencor Alpha Step IQ, and the surface resistance was measured using a surface resistance measuring instrument ("HIRESTA" manufactured by Dia Instruments Co., Ltd.). The results are shown in Table 1.
Figure JPOXMLDOC01-appb-T000001
　表１の結果から明らかなとおり、本発明のブラックマトリックス用カーボンブラック（実施例１及び２）は、染料被覆なしのカーボンブラック（比較例１）と比べて極めて高い表面抵抗が得られると共に、従来の樹脂被覆カーボンブラック（比較例２）と比べて極めて高いＯＤ値が得られることがわかった。 As is clear from the results in Table 1, the carbon black for black matrix of the present invention (Examples 1 and 2) has an extremely high surface resistance as compared with the carbon black without dye coating (Comparative Example 1). It was found that an extremely high OD value was obtained as compared with the resin-coated carbon black (Comparative Example 2).
　上述したように、本発明のブラックマトリックス用カーボンブラックは、高い絶縁性と優れた隠蔽性を備えているので、液晶表示装置等のカラーフィルターのブラックマトリックスに利用した場合極めて有用である。 As described above, since the carbon black for black matrix of the present invention has high insulating properties and excellent concealing properties, it is extremely useful when used for a black matrix of a color filter such as a liquid crystal display device.

Claims (16)

  1. 　カーボンブラックの表面が染料で被覆されてなる、ブラックマトリックス用カーボンブラック。 ¡Carbon black for black matrix with carbon black surface coated with dye.
  2. 　前記染料の含有率が、０．５～１０重量％である、請求項１に記載のブラックマトリックス用カーボンブラック。 The carbon black for black matrix according to claim 1, wherein the content of the dye is 0.5 to 10% by weight.
  3. 　前記染料は、陰イオン性又は非イオン性の染料である、請求項１又は２に記載のブラックマトリックス用カーボンブラック。 The carbon black for black matrix according to claim 1 or 2, wherein the dye is an anionic or nonionic dye.
  4. 　前記染料は、濃色系の染料である、請求項１乃至３の何れか１項に記載のブラックマトリックス用カーボンブラック。 The carbon black for a black matrix according to any one of claims 1 to 3, wherein the dye is a dark color dye.
  5. 　前記染料は、金属又は金属塩によりレーキ化されている、請求項１乃至４の何れか１項に記載のブラックマトリックス用カーボンブラック。 The black dye for black matrix according to any one of claims 1 to 4, wherein the dye is laked with a metal or a metal salt.
  6. 　前記金属又は金属塩は、アルミニウム、マグネシウム、カルシウム、ストロンチウム、バリウム若しくはマンガン又はこれらの塩である、請求項５に記載のブラックマトリックス用カーボンブラック。 The carbon black for a black matrix according to claim 5, wherein the metal or metal salt is aluminum, magnesium, calcium, strontium, barium, manganese, or a salt thereof.
  7. 　前記カーボンブラックは、表面に少なくとも１種類の酸性官能基を有する、請求項１乃至６の何れか１項に記載のブラックマトリックス用カーボンブラック。 The carbon black for a black matrix according to any one of claims 1 to 6, wherein the carbon black has at least one kind of acidic functional group on a surface thereof.
  8. 　前記酸性官能基は、水酸基、オキソ基、ヒドロペルオキシ基、カルボニル基、カルボキシル基、ペルオキシカルボン酸基、アルデヒド基、ケトン基、ニトロ基、ニトロソ基、アミド基、イミド基、スルホン酸基、スルフィン酸基、スルフェン酸基、チオカルボン酸基、クロロシル基、クロリル基、ペルクロリル基、ヨードシル基又はヨージル基である、請求項７に記載のブラックマトリックス用カーボンブラック。 The acidic functional group is a hydroxyl group, oxo group, hydroperoxy group, carbonyl group, carboxyl group, peroxycarboxylic acid group, aldehyde group, ketone group, nitro group, nitroso group, amide group, imide group, sulfonic acid group, sulfinic acid. The carbon black for a black matrix according to claim 7, which is a group, a sulfenic acid group, a thiocarboxylic acid group, a chlorosyl group, a chloryl group, a perchloryl group, an iodosyl group or an iodyl group.
  9. 　カーボンブラックのスラリーに染料を添加して、カーボンブラックの表面を染料で被覆する染料被覆工程を有する、ブラックマトリックス用カーボンブラックの製造方法。 A method for producing carbon black for a black matrix, comprising a dye coating step of coating a surface of carbon black with a dye by adding a dye to a slurry of carbon black.
  10. 　前記染料被覆工程は、得られる染料被覆カーボンブラック中の前記染料の含有率が０．５～１０重量％となるように前記染料を添加することを特徴とする、請求項９に記載のブラックマトリックス用カーボンブラックの製造方法。 The black matrix according to claim 9, wherein in the dye coating step, the dye is added so that the content of the dye in the resulting dye-coated carbon black is 0.5 to 10% by weight. Carbon black manufacturing method.
  11. 　前記染料は、陰イオン性又は非イオン性の染料である、請求項９又は１０に記載のブラックマトリックス用カーボンブラックの製造方法。 The method for producing carbon black for a black matrix according to claim 9 or 10, wherein the dye is an anionic or nonionic dye.
  12. 　前記染料は、濃色系の染料である、請求項９乃至１１の何れか１項に記載のブラックマトリックス用カーボンブラックの製造方法。 The method for producing carbon black for a black matrix according to any one of claims 9 to 11, wherein the dye is a dark-colored dye.
  13. 　前記染料被覆工程で得られた染料被覆カーボンブラック表面の染料を金属又は金属塩によりレーキ化する染料レーキ化工程を更に有する、請求項９乃至１２の何れか１項に記載のブラックマトリックス用カーボンブラックの製造方法。 The carbon black for a black matrix according to any one of claims 9 to 12, further comprising a dye lake step in which the dye on the surface of the dye-coated carbon black obtained in the dye coating step is laked with a metal or a metal salt. Manufacturing method.
  14. 　前記金属又は金属塩は、アルミニウム、マグネシウム、カルシウム、ストロンチウム、バリウム若しくはマンガン又はこれらの塩である、請求項１３に記載のブラックマトリックス用カーボンブラックの製造方法。 The method for producing carbon black for a black matrix according to claim 13, wherein the metal or metal salt is aluminum, magnesium, calcium, strontium, barium, manganese, or a salt thereof.
  15. 　前記染料被覆工程に供する前記カーボンブラックの表面を酸化剤で酸化処理する酸化処理工程を更に有する、請求項９乃至１４の何れか１項に記載のブラックマトリックス用カーボンブラックの製造方法。 The method for producing carbon black for a black matrix according to any one of claims 9 to 14, further comprising an oxidation treatment step of oxidizing the surface of the carbon black subjected to the dye coating step with an oxidizing agent.
  16. 　前記酸化剤は、オゾンガス、硝酸、次亜塩素酸ナトリウム、過酸化水素、一酸化窒素ガス、二酸化窒素ガス、無水硫酸、フッ素ガス、濃硫酸、硝酸又は各種過酸化物である、請求項１５に記載のブラックマトリックス用カーボンブラックの製造方法。 The said oxidizing agent is ozone gas, nitric acid, sodium hypochlorite, hydrogen peroxide, nitrogen monoxide gas, nitrogen dioxide gas, sulfuric anhydride, fluorine gas, concentrated sulfuric acid, nitric acid, or various peroxides. The manufacturing method of carbon black for black matrices as described.
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