WO2004094537A1 - 改質カーボンブラック分散液及びそれを含有する水性インキ - Google Patents
改質カーボンブラック分散液及びそれを含有する水性インキ Download PDFInfo
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- WO2004094537A1 WO2004094537A1 PCT/JP2004/005908 JP2004005908W WO2004094537A1 WO 2004094537 A1 WO2004094537 A1 WO 2004094537A1 JP 2004005908 W JP2004005908 W JP 2004005908W WO 2004094537 A1 WO2004094537 A1 WO 2004094537A1
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- carbon black
- modified carbon
- dispersion
- ink
- water
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/324—Inkjet printing inks characterised by colouring agents containing 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/16—Writing inks
- C09D11/17—Writing inks characterised by colouring agents
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
Definitions
- the present invention relates to a dispersion liquid in which a modified carbon black is dispersed, and a water-based ink containing the same, which is used for a recording liquid, a writing instrument, and the like.
- Carbon black is widely used as a colorant for aqueous inks that print black using an ink jet printer.
- the raw material of carbon black is a secondary aggregate called agglomerate formed by agglomerates, which are primary aggregates of approximately spherical primary particles aggregated, formed by van der Waals force, simple aggregation, adhesion, entanglement, etc. It has become. Such raw carbon black powder immediately settles without being dispersed in water if left untreated.
- a water-based ink containing a raw carbon black powder and a dispersant for dispersing the same in water is difficult to print because of its high viscosity. Therefore, a modified carbon black in which the surface of the raw carbon black is oxidized to introduce a hydrophilic functional group such as a carboxyl group so that the raw carbon black powder can be easily dispersed in water without using a dispersant. Is used.
- Patent Document 1 the specific surface area and the DBP oil absorption (the amount of dimethyl phthalate absorbed by 100 g of carbon black). Disclose something.
- Patent Document 1 Japanese Patent Application Laid-Open No.
- the aqueous ink containing the modified carbon black has a low viscosity and a high print density value, so that deep black and deep printing can be performed.
- the water-based ink must have practically sufficient stability over time when used as a recording ink for an ink jet.
- Conventional aqueous inks increase in viscosity after a long period of time, In some cases, the storage stability was not always sufficient because the carbon black particles were further aggregated and tended to settle. Therefore, there has been a demand for a water-based ink which has a lower sedimentation rate and is less likely to be clogged. Disclosure of the invention
- the present invention has been made to solve the above-mentioned problems, and is used for ink jet printer printing, has a low sedimentation rate, is hardly clogged, and does not increase in viscosity or carbon black particle diameter, and is stable for a long time. It is an object of the present invention to provide a water-based ink that can be stored and stored, and that prints with a deep black and a high print density, and a dispersion of a modified car pump rack used for preparing the ink.
- the present invention relates to a liquid in which a modified carbon black obtained by oxidizing a raw carbon black powder is dispersed, wherein the modified carbon black has a carboxyl group on its surface and 0.8 to 1.1 times that of a carboxyl group.
- the dispersion liquid of the modified carbon black of the present invention made in order to achieve the above object is a dispersion liquid of the modified carbon black obtained by subjecting a raw carbon black powder to an appropriate degree of oxidation treatment.
- lactone groups and carboxyl groups are further introduced into the surface of the raw carbon black powder by this oxidation treatment.
- the modified carbon black has a carboxyl group on the surface and a molar ratio of 0.8 to 1.1 times, preferably 0.85 to 1.05 times, more preferably 0.9 to 1.0 times. And more than 500 ⁇ 1 / g, preferably at least 600 ⁇ 1 / g, more preferably 700 to 90 ⁇ m, in terms of moles per weight of the modified carbon black. 0 ⁇ lZg rataton group.
- the number of carboxyl groups on the surface of the modified carbon black may be at least 700 ⁇ mo 1 / g, preferably 700 to 900 1110 1 Zg. It has a carboxyl group or a rataton group which is a hydrophilic functional group in the above range.
- a large electrostatic repulsion acts between the molecules, and in combination with the relatively large number of lactone groups, it is difficult for the modified carbon black to aggregate.
- the modified carbon black has a hydrophilic functional group and therefore has a strong interaction with water.
- Carboxyl groups and lactone groups are present on the carbon black surface at an appropriate ratio, so that it is easily dispersed in water and sedimented. It is difficult and stable.
- the modified carbon black can be dispersed and Z or dissolved in water without a dispersant.
- Water is added to the modified carbon black or concentrated after that, whereby a dispersion having a desired modified carbon black concentration can be prepared.
- the dispersion may be added, if necessary, to any suitable water-soluble organic solvents and additives such as preservatives.
- the dispersion of the modified carbon black has excellent stability with temperature change. Even after 5 weeks at 70 ° C., the average particle diameter change rate is preferably 15% or less, more preferably 10% or less. The above rate of change is particularly problematic when the change that increases the average particle size is significant.
- the dispersion of the reformed car pump rack does not change in viscosity, and is excellent in stability.
- the viscosity change rate is preferably 10% or less even after 5 weeks at 70 ° C. The rate of change is particularly problematic when the change in viscosity increases is significant.
- the bulk of the car pump rack is manufactured by a known carbon black manufacturing method, and may be carbon black obtained by a furnace method, carbon black obtained by a channel method, or the like. In the furnace method, fuel (gas or oil) and air are introduced into a special combustion furnace lined with bricks that can withstand high temperatures of up to about 200 ° C, and are completely burned.
- the liquid raw material oil is continuously sprayed and thermally decomposed, water is sprayed on the high temperature gas containing carbon black generated in the later stage of the furnace, and the reaction is stopped.
- This is a method for producing raw carbon black powder that separates into black and exhaust gas. According to such a production method, a small amount of lactone groups and carboxyl groups are also introduced into the surface of the raw carbon black powder. This phenomenon, along with the manufacturing method, is deeply related to the shape and surface structure of the car pump rack structure, and this is important for the modified carbon black obtained by oxidizing the raw material powder. It turned out to be a factor.
- the modified carbon black has a carboxyl group and a molar ratio of 0.65 to 1.1 times the molar ratio, and the number of moles per weight of the raw carbon black powder is 20 ⁇ ⁇ ⁇ ⁇ -mo 1 Zg or more. It is preferable that the raw material of the carbon black, which has a group in advance on its surface, is subjected to an oxidation treatment.
- the modified carbon black has a primary particle size (average primary particle size) of 11 to 18 nm and a BET specific surface area of at least 180 m 2 / g, preferably 180 to 260 m 2 Zg.
- the DBP oil absorption (the amount of dibutyl phthalate absorbed by 100 g of the raw carbon black powder: referred to as DBP oil absorption in the present specification) is at least 180 mL / l 00 g, preferably 180 to 3 g. 0
- the layer may be obtained by subjecting a carbon black bulk powder (preferably 190 to 25 OmL / 100 g) to an oxidation treatment.
- the modified carbon black obtained from the raw carbon black powder having such a primary particle diameter has a sedimentation rate of a water-based ink containing it of 30% or less even if the average particle diameter is 150 to 250 nm.
- the ink jet printer ejects this water-based ink at a low level, and is unlikely to cause clogging, sedimentation, and deterioration of the nozzles, and exhibits practical long-term storage stability for several years.
- the modified carbon black Since the modified carbon black has good dispersion stability, the sedimentation rate is low even in the carbon black dispersion of the invention and the aqueous ink.
- the sedimentation rate was measured by centrifuging a liquid prepared to a modified carbon black concentration of 5% by weight, diluting the liquid before and after centrifugation, measuring the absorbance at a wavelength of 500 nm, and measuring the change. Expressed as a percentage. Specifically, the measurement is performed as follows.
- the sedimentation rate is calculated by the formula for calculating the absorbance value WO.
- the modified carbon black preferably has a sedimentation rate of 30% or less, preferably 25% or less, obtained as described above.
- the carbon black dispersion containing the modified carbon black having such a sedimentation rate, and the aqueous ink prepared by using the dispersion have an average particle diameter of the modified carbon black within the above range. Even if it is relatively large as described above, it does not settle even after long-term storage for several years and is hardly deteriorated and stable. Also, when this aqueous ink is used for an ink jet printer, printing can be performed smoothly without causing clogging of the ink jet nozzle of the ink jet printer. Further, since the dispersion liquid and the ink have a high OD value, deep black and deep printing can be performed. On the other hand, ink using a car pump rack exhibiting a sedimentation rate exceeding the above range may cause clogging or sedimentation due to long-term storage.
- Examples of the method of oxidizing the raw carbon black powder include: an oxidation method by contact with air; a gas phase oxidation method by reaction with nitrogen oxides and ozone; nitric acid, permanganic acid potassium, potassium dichromate, chlorite, A liquid phase oxidation method using an oxidizing agent such as perchloric acid, hypohalite, hydrogen peroxide, a bromine aqueous solution, or an ozone aqueous solution may be used.
- the surface may be modified by plasma treatment or the like.
- a particularly preferred oxidation method is a method of wet oxidation of raw carbon black powder using hypohalous acid or a salt thereof.
- hypohalite include sodium hypochlorite and hypochlorous acid, and sodium hypochlorite is more preferable from the viewpoint of reactivity.
- the carbon black dispersion is produced, for example, by adding an aqueous solution of hypohalous acid or Z and hypohalous acid to a liquid obtained by suspending the bulk of a car pump rack prepared by the furnace method in water, and oxidizing the solution. After processing, a modified carbon black was obtained and stirred with a milling medium having a diameter of 0.6 to 3 mm using a dispersing machine to obtain 100 to 500 At least a step of filtering off with a mesh wire mesh and desalting the filtrate with an ultrafiltration membrane is provided, whereby a dispersion is obtained.
- hypohalous acid or a salt thereof preferably sodium hypochlorite as an oxidizing agent
- the surface of the raw carbon black powder is oxidized, and rataton groups and carboxyl groups are introduced.
- the amount of hypohalous acid or a salt thereof used is appropriately adjusted according to the BET specific surface area of the raw carbon black powder.
- the smaller the BET specific surface area the smaller the number of active sites reacting with hypohalous acid, and the larger the specific surface area, the more active sites react with hypohalogenous acid.
- Addition of hypohalous acid in an amount greater than the amount that reacts with the active site does not hinder the reaction, but wasteful hypohalous acid is used, and an extra desalting operation is required.
- the reaction is performed with an amount of hypohalous acid below the amount that reacts with the active site, the target amount of rataton groups and carboxyl groups will not be reached, and the sedimentation rate will increase, resulting in a decrease in long-term storage stability. I will.
- the dispersion may be carried out using a disperser or a high-speed stirrer with a high load.
- a water-soluble solvent may be previously infiltrated into carbon black.
- a pole mill, attritor, hooded jet mixer, impeller mill, colloidal as a disperser or pulverizer Mill, sand mill for example, "super mill", Gitator mill “,” Dyno mill “, and” beads mill “).
- the mill medium is not necessarily used, but is preferably used.
- the mill medium preferably has a diameter of 0.6 to 3 mm, and specific examples include glass beads, zircon beads, magnetic beads, and stainless steel beads.
- the conditions in the step of dispersing while oxidizing are preferably 10 to 70 hours and 3 to 10 hours, and the rotation speed is preferably 500 rpm or more.
- the oxidation reaction proceeds more easily as the reaction temperature is higher. However, if the temperature is too high, the hypohalite is decomposed. Therefore, the oxidation reaction is preferably performed at 40 to 60 ° C.
- Filtration through wire mesh is performed to remove coarse particles and mill media.
- the pH of the obtained filtrate may be adjusted.
- the excess acid or by-produced water-soluble acid group in the obtained filtrate may be neutralized with a basic substance.
- basic substances include hydroxides of alkali metal, such as sodium hydroxide, hydroxide hydroxide and lithium hydroxide; ammonia and aqueous ammonia; amine compounds.
- the amine compound include a water-soluble volatile amine and alkanolamine.
- volatile amines substituted with an alkyl group having 1 to 3 carbon atoms eg, methylamine, trimethylamine, getylamine, propylamine
- alkanols substituted with an alkyl group having 1 to 3 carbon atoms Amines (eg, ethanolamine, diethanolamine, triethanolamine, triisopropanolamine); alkyl / recanolamines substituted with an alkyl group having 1 to 3 carbon atoms or an alkanol group having 1 to 3 carbon atoms.
- the desalting method may be a combination of various desalting methods. A pigment dispersion desalted by the above method can be obtained.
- the modified carbon black obtained from such a desalted dispersion has an electric conductivity of 0.7 mS / cm or less, so that an ink having good storage stability can be prepared. Can be used for
- the dispersion may be obtained by further removing coarse particles of 1 ⁇ or more using a centrifuge or a filter. Coarse particles are likely to settle, increase the settling rate, and may cause clogging of the ink ejection nozzle of the ink jet printer.
- the aqueous ink of the present invention contains the modified carbon black dispersion.
- the water-based ink contains a modified carbon black, so it can be printed clearly and deeply in black with deep and clear, has good storage stability, and is unlikely to cause sedimentation even when stored for a long time.
- the modified carbon black is contained in an amount of 0.1 to 20% by weight, preferably 1 to 15% by weight, based on the total amount of the aqueous ink. If the content of the modified carbon black is less than 0.1% by weight, the printing or writing density may be insufficient. If it exceeds 20% by weight, the viscosity of the water-based ink sharply increases, and The stability at the time of ejection may decrease.
- the water-based ink may have a permeability such that the permeation time is less than 1 second when the applied amount of the ink to a recording medium exemplified by paper is 1 mg "cm ⁇ 2 >.
- An ink that has a permeation time of less than 1 second at 1 mg Z cm 2 is, for example, 50 ng of water-based ink in an area of 360 dpi (dot Z inch) x 360 dpi. When applied, it refers to an aqueous ink that takes less than 1 second to remove the stain with the ink even when touching the printed surface.
- a penetration enhancer such as a water-soluble organic solvent or a surfactant that reduces the surface tension of the aqueous solution is added to the ink according to the recording medium.
- a penetration enhancer such as a water-soluble organic solvent or a surfactant that reduces the surface tension of the aqueous solution is added to the ink according to the recording medium.
- water-soluble organic solvent examples include lower alcohols such as ethanol and propanol; cellosonoles such as ethylene glycol monomethyl ether and ethylene glycol monoethyl ether; and carbiols such as diethylene glycol monomethyl ether monoethyl ether and ethylene glycol monoethyl ether.
- Surfactants include, for example, anionic surfactants such as fatty acid salts and alkyl sulfate salts; nonionic surfactants such as polyoxyethylene alkyl ether and polyoxyethylene ether; cationic surfactants; And an on-active surfactant.
- anionic surfactants such as fatty acid salts and alkyl sulfate salts
- nonionic surfactants such as polyoxyethylene alkyl ether and polyoxyethylene ether
- cationic surfactants such as polyoxyethylene alkyl ether and polyoxyethylene ether
- cationic surfactants such as polyoxyethylene alkyl ether and polyoxyethylene ether
- an on-active surfactant such as fatty acid salts and alkyl sulfate salts
- nonionic surfactants such as polyoxyethylene alkyl ether and polyoxyethylene ether
- cationic surfactants such as polyoxyethylene alkyl ether and polyoxyethylene ether
- cationic surfactants such as poly
- a water-soluble organic solvent and a surfactant may be used alone or in combination.
- the penetration enhancer is preferably added to the aqueous ink while adjusting the surface tension of the aqueous ink at 20 ° C. to be 45 mN nom or less, preferably 4 OmNZm or less.
- a humectant may be added to the aqueous ink to prevent the ink from drying at the tip of the nozzle that discharges the ink when used for ink jet recording.
- the humectant is selected from water-soluble and highly hygroscopic materials.
- glycerin ethylene glycolone, diethylene glycolone, triethylene glycolone, polyethylene glycol, propylene glycolone, dipropylene glycol, polypropylene glycol, 1,3-propanoldiol, 1,4-butanediol
- Polyols such as diol, 1,5-pentanediole, 1,6-hexanediol, 1,2,6-hexanetriol and pentaerythritol; 2-pyrrolidone, N-methyl-2-pyrrolidone, ⁇ - Ratatams such as caprolactam; ureas such as urea, thiourea, ethylene urea, 1,3-dimethylimidazolidinone; saccharides such as maltitol, sorbitol, darconolatatone, and maltose.
- the amount of the humectant is not particularly limited, but is generally in the range of 0.5 to 5 0 wt
- additives such as a fixing agent, a ⁇ adjuster, an antioxidant, an ultraviolet absorber, a preservative, and a fungicide may be added to the aqueous ink.
- Water-based ink is, for example, modified carbon black concentration of 5 wt%, glycerin 1 0 wt 0/0, adjusted to diethylene one mono- ⁇ - butyrate Honoré ether 1 0 wt% It was made.
- this aqueous ink is applied at 1 mg / cm 2, the reflection density value (OD value) of the ink layer measured by a Macbeth densitometer is at least 1.4.
- This water-based ink is preferably used as an ink for which long-term stability is required, for example, as an ink for ink jet recording in which ink droplets are ejected and adhered to a recording medium, and for writing implements, stamps, and the like. It is also used as various inks such as A water-based ballpoint pen using this water-based ink as a writing ink composition has good recording and writing characteristics, enables writing without unevenness in handwriting, and does not blur characters even when short-handed.
- recording is performed on a recording medium by adhering ink.
- This recording method may be an ink jet recording method in which droplets of aqueous ink are ejected, and the droplets are attached to a recording medium to perform printing.
- an aqueous ink is ejected as droplets from a fine nozzle, and the droplets are attached to a recording medium by various methods.
- the first method is an electrostatic suction method.
- a strong electric field is applied between the nozzle and an accelerating electrode placed in front of the nozzle, ink is continuously ejected from the nozzle in the form of droplets, and the ink droplets fly between the deflecting electrodes.
- a printing information signal is applied to a deflection electrode for recording, or a method in which an ink droplet is ejected in accordance with the printing information signal without being deflected.
- the second method is a method in which ink is forcibly ejected by applying pressure to the ink liquid with a small pump and mechanically vibrating the nozzle with a crystal oscillator or the like. It is charged, and a printing information signal is applied to the deflection electrode while the ink droplet flies between the deflection electrodes, and recording is performed.
- the third method is a method using a piezoelectric element, in which pressure and a print information signal are simultaneously applied to the ink by the piezoelectric element to eject and record ink droplets.
- the fourth method is to expand the volume of the ink rapidly by the action of thermal energy.
- the ink is heated and foamed with microelectrodes according to the print information signal, and the ink droplets are ejected and recorded.
- the ink jet recording method may be performed by any method.
- the recorded matter of the present invention is obtained by performing recording using an aqueous ink.
- the printed matter is printed with high density, deep black color, and is clear and clear.
- Examples 1 to 3 show examples of preparing a dispersion of modified carbon black to which the present invention is applied.
- the reaction solution was filtered through a 400-mesh wire net to separate the reaction solution from zirconia beads and unreacted carbon black.
- a 5% aqueous solution of potassium hydroxide was added to adjust the pH to 7.5.
- Desalting and purification were performed using an ultrafiltration membrane until the conductivity of the solution reached 1.5 mSZcm.
- the solution was further desalted and purified using an electrodialyzer until the conductivity of the solution reached 1. OmS / cm.
- the solution was concentrated until the concentration of the modified carbon black reached 17% by weight. The concentrate was centrifuged to remove coarse particles, and filtered through a 0.6 ⁇ m filter.
- reaction solution was filtered through a 400-mesh wire gauze to separate the reaction solution from zircon beads and unreacted carbon black.
- a 5% aqueous solution of sodium hydroxide was added to the reaction solution obtained by fractionation to adjust the pH to 7.5.
- Desalting and purification were performed using an ultrafiltration membrane until the conductivity of the liquid reached 1.5 mSZcm.
- the solution was further desalted and purified using an electrodialyzer until the conductivity of the solution reached 1. OmSZcm.
- the solution was concentrated until the concentration of the modified carbon black reached 17% by weight.
- the concentrate was centrifuged to remove coarse particles and filtered through a 0.6 filter. Ion-exchanged water was added to the obtained filtrate, and the mixture was diluted until the concentration of the modified carbon black became 15% by weight, and dispersed to obtain a dispersion B of the modified carbon black.
- the reaction solution was filtered through a 400-mesh wire gauze to separate the reaction solution from glass beads and unreacted carbon black.
- a 5% aqueous solution of sodium hydroxide was added to the reaction solution obtained after the separation to adjust the pH to 7.5. did.
- the solution was desalted and purified with an ultrafiltration membrane until the conductivity of the solution reached 1.5 mSZ cm. Desalting and purification were performed using an electrodialysis device until the conductivity of the solution reached 1. OmS / cm.
- the solution was concentrated until the concentration of the modified carbon black reached 17% by weight.
- the concentrate was centrifuged to remove coarse particles, and filtered through a 0.6 ⁇ filter. Ion-exchanged water was added to the obtained filtrate, and the mixture was diluted until the concentration of the modified carbon black became 15% by weight and dispersed to obtain a dispersion C of the modified carbon black.
- reaction solution containing the modified carbon black.
- This reaction solution was filtered through a 400-mesh wire net to separate the reaction solution from zirconia beads and unreacted carbon black.
- a 5% aqueous solution of sodium hydroxide was added to the reaction solution obtained by fractionation to adjust the pH to 7.5.
- the solution was desalted and purified using an ultrafiltration membrane until the conductivity of the solution reached 1.5 mSZcm.
- the solution was concentrated until the concentration of the modified carbon black reached 17% by weight.
- the concentrate was centrifuged to remove coarse particles, and filtered through a 0.6 m filter. Ion-exchanged water was added to the obtained filtrate to dilute and disperse the modified carbon black until the concentration of the modified carbon black became 15% by weight to obtain a dispersion D of the modified car pump rack.
- the reaction solution was filtered through a 400-mesh wire net to separate the reaction solution from zirconia beads and unreacted carbon black.
- a 5% aqueous solution of sodium hydroxide was added to the reaction solution obtained by fractionation to adjust the pH to 7.5.
- the solution was desalted and purified using an ultrafiltration membrane until the conductivity of the solution reached 1.5 mS / cm.
- the resulting solution has a modified carbon black concentration of 17% by weight. Concentrated to / 0 .
- the concentrate was centrifuged to remove coarse particles, and filtered with a 0.6 filter. Ion-exchanged water was added to the obtained filtrate, and the modified carbon black was diluted to a concentration of 15% by weight and dispersed to obtain a dispersion E of carbon black.
- the mixture was pulverized by a sand mill for 30 minutes to obtain a reaction liquid containing the modified carbon black.
- the reaction solution was filtered through a 400 mesh wire mesh to separate the reaction solution from zirconia beads and unreacted carbon black.
- a 5% aqueous solution of sodium hydroxide was added to the reaction solution obtained after the separation to adjust the pH to 7.5, and then desalting and purification were performed with an ultrafiltration membrane until the conductivity reached 1.5 mS / cm.
- the solution was concentrated until the concentration of the modified carbon black reached 17% by weight.
- the concentrated solution was centrifuged to remove coarse particles, and filtered through a 0.6 ⁇ Hi filter. To the resulting filtrate was added ion-exchanged water, diluted until the concentration of the modified carbon black became 15% by weight, and dispersed to obtain a dispersion F of carbon black.
- reaction solution containing the modified carbon black.
- This reaction solution was filtered through a 400 mesh wire mesh to separate the reaction solution from zircon beads and unreacted carbon black.
- a 5% aqueous solution of sodium hydroxide was added to the reaction solution obtained after the separation to adjust the pH to 7.5, and then desalting and purification were performed with an ultrafiltration membrane until the conductivity reached 1.5 mSZ cm.
- the solution was concentrated until the concentration in the reformer car pump rack became 17% by weight. This concentrated liquid was centrifuged to remove coarse particles, and filtered with a 0.6 m filter. To the resulting filtrate was added ion-exchanged water, diluted until the concentration of the modified carbon black became 15% by weight, and dispersed to obtain a dispersion G for a car pump rack.
- the obtained modified carbon black was dried at 60 ° C for 15 hours, and the pyrolysis gas chromatograph HP 589 OA was used using the carbon black. (Trade name, manufactured by Hewlett-Packard Co., Ltd.) was used to measure the CO 2 generated by the decomposition of the ratatone group at 358 ° C. and the carboxyl group at 650 ° C. Based on the measured values, the abundance of ratatone groups and carboxyl groups of carbon black was converted.
- the average particle diameter was measured using a particle size analyzer MI CROTRAC 9340-UPA (trade name of Microtrac).
- Table 1 shows the evaluation results.
- the concentration of modified carbon black is 15 weight. / 0 , and the dispersion after leaving it at 70 ° C for 5 weeks, using an E-type viscometer RE 550 L (trade name, manufactured by Toki Sangyo Co., Ltd.). Was measured, and the rate of change was calculated.
- Equation 2 #It is the viscosity of the dispersion after standing—the viscosity of the dispersion before standing v1 nn The rate of change in viscosity (/.) The viscosity of the dispersion before standing Xl ° ° (b) 70 ° C, Measurement of average particle diameter change rate of carbon black before and after standing for 5 weeks Using the dispersion liquid before and after standing at 70 ° C for 5 weeks, the respective average particle diameters were measured by the above method, and the change rates were measured. Calculated.
- Table 2 shows the results of the evaluation.
- Table 3 shows examples of the production of aqueous inks with different ink compositions (H composition and ⁇ composition). As shown in Table 3, the dispersions A to C described above were used for the aqueous inks of the examples, and the dispersions D to G described above were used for the aqueous inks of the comparative examples, as shown in Table 3.
- Aqueous ink composition Preparation of ⁇ composition
- the mixture was filtered with a membrane filter (trade name, manufactured by Millipore) having a pore size of 5 ⁇ m at 20 to prepare a water-based ink.
- a membrane filter (trade name, manufactured by Millipore) having a pore size of 5 ⁇ m at 20 to prepare a water-based ink.
- the sedimentation rate was calculated by the formula for calculating the absorbance value W0.
- the obtained water-based ink was filled into an ink jet recording device EM-900C (trade name, manufactured by Seiko Epson Corporation), and the amount of ink applied was adjusted to l mgZ cm 2.
- EM-900C trade name, manufactured by Seiko Epson Corporation
- Printed on a certain Xerox-1 P (trade name of Fuji Xerox).
- the reflection density value (OD value) was measured with a Macbeth densitometer TR-927 (trade name, manufactured by Cole Mogen).
- Table 3 shows the evaluation results.
- the modified carbon black dispersion of the present invention can be easily produced in large quantities, and the carbon black is homogeneously dispersed in water without using a dispersant or a surfactant. Since the dispersion of the modified carbon black does not require a polymer dispersant, it does not increase the viscosity of the dispersion or the particle size of the carbon black, has good storage stability, and is an aqueous solution requiring long-term stability. It is suitably used for ink.
- the aqueous ink containing the modified carbon black dispersion of the present invention is suitably used for an ink jet printer.
- This ink has good storage stability and hardly sediments when stored for a long period of time, and has a long shelf life. Also, it is difficult to cause clogging of the ink ejection nozzle of the ink jet printer.
- the prints and images have a high print density and are clear, deep and black.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
Description
Claims
Priority Applications (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US10/517,951 US7220304B2 (en) | 2003-04-23 | 2004-04-23 | Modified carbon black dispersion liquid and water base ink containing the same |
EP20040729282 EP1616913B1 (en) | 2003-04-23 | 2004-04-23 | Modified carbon black dispersion liquid and water base ink containing the same |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2003117995A JP4189258B2 (ja) | 2003-04-23 | 2003-04-23 | 改質カーボンブラック分散液及びそれを含有する水性インキ |
JP2003-117995 | 2003-04-23 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2004094537A1 true WO2004094537A1 (ja) | 2004-11-04 |
Family
ID=33308059
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2004/005908 WO2004094537A1 (ja) | 2003-04-23 | 2004-04-23 | 改質カーボンブラック分散液及びそれを含有する水性インキ |
Country Status (5)
Country | Link |
---|---|
US (1) | US7220304B2 (ja) |
EP (1) | EP1616913B1 (ja) |
JP (1) | JP4189258B2 (ja) |
CN (1) | CN100338148C (ja) |
WO (1) | WO2004094537A1 (ja) |
Cited By (1)
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---|---|---|---|---|
US9221986B2 (en) | 2009-04-07 | 2015-12-29 | Sensient Colors Llc | Self-dispersing particles and methods for making and using the same |
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JP2007119512A (ja) * | 2005-10-25 | 2007-05-17 | Seiko Epson Corp | 顔料分散液の製造方法、顔料分散液、インクジェット記録用インク組成物、記録方法、及び記録物 |
WO2008055244A2 (en) | 2006-10-31 | 2008-05-08 | Sensient Colors Inc. | Modified pigments and methods for making and using the same |
US20080249217A1 (en) * | 2007-02-27 | 2008-10-09 | Sze-Ming Lee | Inkjet ink compositions comprising multiple modified pigments |
US8328341B2 (en) * | 2007-07-23 | 2012-12-11 | Canon Kabushiki Kaisha | Ink jet recording ink, ink jet image-forming method and ink jet recording apparatus |
US8328926B2 (en) | 2007-07-23 | 2012-12-11 | Canon Kabushiki Kaisha | Ink jet recording ink, ink jet image-forming method and ink jet recording apparatus |
WO2009026552A2 (en) | 2007-08-23 | 2009-02-26 | Sensient Colors Inc. | Self-dispersed pigments and methods for making and using the same |
JP5353059B2 (ja) * | 2008-05-26 | 2013-11-27 | 株式会社リコー | 画像形成方法 |
JP5787482B2 (ja) * | 2009-01-22 | 2015-09-30 | キヤノン株式会社 | インクジェット記録用インク及びインクジェット画像形成方法 |
JP2010188721A (ja) * | 2009-01-22 | 2010-09-02 | Canon Inc | インクジェット画像形成方法及びインクジェット記録装置 |
EP2456832A1 (en) | 2009-07-24 | 2012-05-30 | E. I. du Pont de Nemours and Company | Self-dispersing pigment dispersions and ink jet inks containing them |
US8388125B2 (en) | 2010-02-24 | 2013-03-05 | Canon Kabushiki Kaisha | Inkjet recording ink |
US8403461B2 (en) | 2010-05-04 | 2013-03-26 | Kabushiki Kaisha Toshiba | Aqueous inkjet ink |
JP5672451B2 (ja) * | 2011-03-10 | 2015-02-18 | 東海カーボン株式会社 | 表面処理カーボンブラック粒子水性分散体の製造方法および表面処理カーボンブラック粒子水性分散体 |
TWI605096B (zh) * | 2012-02-29 | 2017-11-11 | 大同化成工業股份有限公司 | 黑色矩陣用碳黑及其製造方法 |
ITTO20130587A1 (it) | 2012-07-13 | 2014-01-14 | Cabot Corp | Nerofumi altamente strutturati |
CN103031023B (zh) * | 2012-12-20 | 2015-04-29 | 广州市番禺科迪色彩有限公司 | 一种高性价比氧化铁黑水性色浆的制备方法 |
JP6735065B2 (ja) * | 2015-03-13 | 2020-08-05 | セイコーエプソン株式会社 | インクジェット記録装置及び水系インク組成物 |
CN107778531A (zh) * | 2017-11-17 | 2018-03-09 | 青岛黑猫炭黑科技有限责任公司 | 一种炭黑干法处理制备浆液的方法 |
KR102477024B1 (ko) * | 2017-12-27 | 2022-12-12 | 오씨아이 주식회사 | 고저항성 카본 블랙의 제조방법 및 이에 따라 제조된 고저항성 카본블랙 |
CN109976114A (zh) * | 2019-03-05 | 2019-07-05 | 湖北雨田科技有限公司 | 一种印刷用耐储存彩色墨粉及其制备方法 |
CN114574005B (zh) * | 2022-01-22 | 2023-01-17 | 德欣精细化工(深圳)有限公司 | 一种化纤着色炭黑及其制备方法 |
CN116382032B (zh) * | 2023-02-07 | 2023-09-22 | 万思得新材料科技(中山)有限公司 | 一种适用于lcd光刻胶的高稳定性黑色纳米分散液 |
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JPS61919A (ja) * | 1984-06-13 | 1986-01-06 | Hitachi Maxell Ltd | 磁気記録媒体 |
JP2000345086A (ja) * | 1999-06-09 | 2000-12-12 | Seiko Epson Corp | 水性インク組成物 |
JP2000345085A (ja) * | 1999-06-09 | 2000-12-12 | Seiko Epson Corp | 水性インク組成物 |
WO2000075246A1 (en) * | 1999-06-09 | 2000-12-14 | Orient Chemical Industries, Ltd. | Aqueous pigment dispersion and process for producing the same |
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DE2654598B2 (de) * | 1976-12-02 | 1979-01-25 | Hoechst Ag, 6000 Frankfurt | In hydrophoben und hydrophilen Medien leicht verteilbare, flockungsstabile Feststoffdispersionen und ihre Verwendung |
JPS6122424A (ja) * | 1984-07-09 | 1986-01-31 | Hitachi Maxell Ltd | 磁気記録媒体 |
JPS63144122A (ja) * | 1986-12-03 | 1988-06-16 | Sumitomo Metal Ind Ltd | 塩酸酸洗廃液からけい素を除去する方法 |
US5609671A (en) * | 1994-06-20 | 1997-03-11 | Orient Chemical Industries, Ltd. | Water-based pigment ink and process for producing the same |
IL154538A (en) * | 1994-12-15 | 2009-12-24 | Cabot Corp | The reaction of carbon black with diazonium salts, the resulting carbon black products |
DE69623158T2 (de) * | 1995-03-20 | 2003-04-30 | Orient Chemical Ind | Verfahren zur Herstellung einer wässrigen pigmenthaltigen Tinte |
EP0851412B1 (en) * | 1996-12-27 | 2007-03-07 | TDK Corporation | Magnetic recording medium |
JP2000319573A (ja) | 1999-03-10 | 2000-11-21 | Seiko Epson Corp | 水性顔料分散液、水性インク組成物および前記インク組成物を用いた記録方法 |
JP3749406B2 (ja) | 1999-09-17 | 2006-03-01 | 東海カーボン株式会社 | 水性インキ用カーボンブラック顔料 |
WO2004061015A1 (ja) * | 2002-12-27 | 2004-07-22 | Seiko Epson Corporation | 改質カーボンブラック,カーボンブラック分散液及び水性インキ |
-
2003
- 2003-04-23 JP JP2003117995A patent/JP4189258B2/ja not_active Expired - Fee Related
-
2004
- 2004-04-23 EP EP20040729282 patent/EP1616913B1/en not_active Expired - Fee Related
- 2004-04-23 CN CNB2004800003894A patent/CN100338148C/zh not_active Expired - Fee Related
- 2004-04-23 US US10/517,951 patent/US7220304B2/en not_active Expired - Lifetime
- 2004-04-23 WO PCT/JP2004/005908 patent/WO2004094537A1/ja active Application Filing
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61919A (ja) * | 1984-06-13 | 1986-01-06 | Hitachi Maxell Ltd | 磁気記録媒体 |
JP2000345086A (ja) * | 1999-06-09 | 2000-12-12 | Seiko Epson Corp | 水性インク組成物 |
JP2000345085A (ja) * | 1999-06-09 | 2000-12-12 | Seiko Epson Corp | 水性インク組成物 |
WO2000075246A1 (en) * | 1999-06-09 | 2000-12-14 | Orient Chemical Industries, Ltd. | Aqueous pigment dispersion and process for producing the same |
Non-Patent Citations (1)
Title |
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See also references of EP1616913A4 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9221986B2 (en) | 2009-04-07 | 2015-12-29 | Sensient Colors Llc | Self-dispersing particles and methods for making and using the same |
Also Published As
Publication number | Publication date |
---|---|
CN100338148C (zh) | 2007-09-19 |
EP1616913A4 (en) | 2011-03-09 |
JP4189258B2 (ja) | 2008-12-03 |
US7220304B2 (en) | 2007-05-22 |
EP1616913A1 (en) | 2006-01-18 |
CN1697860A (zh) | 2005-11-16 |
US20050204957A1 (en) | 2005-09-22 |
JP2004346090A (ja) | 2004-12-09 |
EP1616913B1 (en) | 2014-09-03 |
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