JP2006321821A - Method for producing pigment - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To solve problems of restriction of a production scale, dispersion of quality every lot, mixing-in of foreign material because of open type, contamination, etc. of operation environment by occurrence of powder dust cited as subjects in conventional batch type kneaders, etc. <P>SOLUTION: The method for producing a pigment comprises kneading a mixture of an organic pigment with a water-soluble inorganic salt in an amount of ≥7 pts.wt. and ≤30 pts.wt. based on 1 pt.wt. organic pigment and a water-soluble organic liquid in an amount of ≥0.3 pt.wt. and ≤7 pts.wt. based on 1 pt.wt. organic pigment by a continuous kneading machine having crushing spaces formed at the gaps between circular stationary disks and rotary disks coaxial to the stationary disks and integrally rotating around the axis of a driving shaft. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a method for producing a pigment in which particles of color developing powder are finely sized to have a uniform particle size and extremely dispersible with respect to a vehicle. More specifically, in the present invention, when particles of coloring powder are dispersed in a printing ink such as gravure ink or offset ink or a vehicle such as paint, the developed product is given good gloss and high coloring power, Further, the present invention relates to a method for producing a pigment that gives excellent suitability even in applications requiring finer pigment particles such as inkjet inks and color filters.

  Some organic pigments, such as azo pigments, can obtain finely sized particles by selecting appropriate reaction conditions during synthesis. In addition, very fine and agglomerated particles produced during synthesis such as chlorinated copper phthalocyanine pigments are grown and sized in the subsequent process, and coarse and irregular particles produced during synthesis such as copper phthalocyanine pigments are used later. Some perform processing called pigmentation, which is refined and sized in the process.

For example, copper phthalocyanine pigments are used in large quantities and widely in the field of color material industry because of their beautiful color tone, high tinting strength, and good performance such as weather resistance and heat resistance.
Usually, a copper phthalocyanine pigment is an alkylbenzene in the presence or absence of a catalyst such as ammonium molybdate or titanium tetrachloride, or phthalodinitrile or a derivative thereof and urea and a copper source, or phthalodinitrile or a derivative thereof and a copper source. , By reacting in an organic solvent such as trichlorobenzene or nitrobenzene at normal pressure or under pressure.
However, the synthesized phthalocyanine molecules can be obtained only in coarse and needle-like particles having a major axis of about 10 to 200 μm by causing particle growth one after another in the synthesis solvent, such as inks, paints, plastics, etc. As a coloring pigment, the value is very low and it is called crude copper phthalocyanine. Therefore, it is necessary to refine the crude copper phthalocyanine to particles having high utility value in color, that is, about 0.01 to 0.5 μm.

  There are various known examples of methods for industrially refining crude copper phthalocyanine, such as ball mills and attritors obtained by adding a small amount of solvent such as diethylene glycol to a mixture of crude copper phthalocyanine and sodium chloride and then wetting it. In addition, there is a so-called solvent salt milling method in which a kneader is kneaded strongly with a batch kneader or the like and is wet ground (see Patent Document 1). In this method, sodium chloride, diethylene glycol and the like are removed from the obtained kneaded product by washing with water and dried to obtain a copper phthalocyanine pigment with fine primary particles.

However, conventional batch type kneaders have problems such as production scale limitations derived from the batch type, variation in quality for each lot, contamination of the work environment due to foreign matter contamination and dust generation due to the open type.
In addition, there is a limit to the use of enormous energy for the miniaturization of organic pigments and the level of miniaturization. Furthermore, even when the obtained copper phthalocyanine pigment is used dispersed in a vehicle such as gravure ink, offset ink or printing ink or paint, improvement of gloss and coloring power is always a required issue. there were.

Japanese Patent Laid-Open No. 7-53889

The present invention has been made in view of such a situation, and is due to restrictions on production scale, variations in quality for each lot, problems due to the open type, contamination by foreign matter, and generation of dust. It aims at providing the manufacturing method of the pigment which solves the pollution of a working environment, etc.

  Furthermore, the present invention can obtain finer particles with a small amount of energy as compared with conventional batch kneaders, etc., and is dispersed in a vehicle such as gravure ink, offset ink or printing ink or paint. Produces pigments that, when used, give good extensibility and color strength to developed products, and give excellent suitability even in applications that require finer pigment particles such as inkjet inks and color filters. It aims to provide a method. That is, an object of the present invention is to provide a method for efficiently producing a fine pigment that cannot be obtained by a conventional batch kneader or the like in a short time.

  The present invention comprises an organic pigment, a water-soluble inorganic salt of 7 to 30 times by weight of the organic pigment, and a water-soluble organic liquid of from 0.3 to 7 times by weight of the organic pigment. The mixture is kneaded in a continuous kneader having a pulverization space formed in a gap portion between an annular fixed disk and the fixed disk that rotates integrally around the axis of the drive shaft and the concentric rotating disk. This is a method for producing a pigment.

  By adopting such a configuration, the production scale is less restricted than a conventional batch kneader and the like, and timely and appropriate quantity production is possible, and there is little variation in the quality of each product lot. Moreover, since it becomes a sealed type, problems such as contamination of the work environment due to generation of dust and contamination of foreign matters are solved. In addition, when the pigment can be pulverized to finer particles with a small amount of energy, or when the organic pigment obtained from this production method is dispersed in a printing ink such as gravure ink or offset ink or a vehicle such as paint, the pigment is Good gloss and improvement in coloring power are imparted to a color product, and excellent aptitude is also obtained in applications requiring finer pigment particles such as inkjet inks and color filters. In addition, it is possible to easily produce a fine pigment that cannot be obtained by a conventional batch kneader or the like in a short time.

  Further, the water-soluble inorganic salt is less than 7 times by weight because the water-soluble inorganic salt is 7 to 30 times by weight and the water-soluble organic liquid is from 0.3 to 7 times by weight with respect to the organic pigment. In some cases, the inconvenience of being difficult to miniaturize is solved, and in the case of 30 times by weight or more, it is possible to obtain a finer pigment, but since the amount of pigment processing decreases, the productivity is lowered and industrially reduced. The disadvantage of being disadvantageous is resolved. In other words, finer organic pigments are produced by solvent salt milling with respect to organic pigments under conditions where the amount of water-soluble inorganic salt used is higher than in the past. In addition, when the water-soluble organic liquid is less than 0.3 times by weight, the inconvenience that the kneaded composition becomes too hard and difficult to operate stably is solved, and when it is more than 7 times by weight, the kneaded composition becomes soft. The inconvenience that the fineness level is lowered after that is eliminated.

  The invention according to claim 2 is characterized in that, in the invention according to claim 1, the kneading temperature is controlled to 10 to 150 ° C. By adopting such a configuration, both the grinding of organic pigment particles and the growth of organic pigment particles by contact with a water-soluble organic solvent effectively proceed.

According to the first aspect of the invention, it is possible not only to contribute to the improvement of the working environment and the prevention of foreign matter from being mixed into the product, while ensuring the reduction of the equipment cost and the manufacturing cost. When dispersed in a vehicle such as gravure ink, offset ink, or other printing ink or paint, it is possible to improve the gloss and coloring power of the developed product. Furthermore, by increasing the amount of the water-soluble inorganic salt from conditions such as a conventional batch kneader, the organic pigment can be made finer and finer, and the productivity can be improved. It can contribute to the stable operation of continuous production.
According to the second aspect of the present invention, both the grinding of the organic pigment particles and the particle growth of the organic pigment due to contact with the water-soluble organic solvent can be effectively advanced.

First, a continuous kneader used for carrying out the method of the present invention will be described with reference to FIG. FIG. 1 is a side sectional view showing an embodiment of a continuous kneader according to the present invention. Incidentally, the continuous kneader suitably used in the present invention is described in Japanese Patent Publication No. 2-92, etc., for example, a continuous kneader 10 ("Miracle K.C." .K. ") Can be mentioned as preferred.
As shown in FIG. 1, the continuous kneader 10 has a basic configuration including a feed unit 1, a kneading unit 2, a discharge unit 3, and a quantitative feeder unit 4. The feed portion 1 includes a cylindrical casing 11 that extends in the horizontal direction, and a spiral rod 12 that is concentrically fitted into the casing 11 and is fitted in a sliding contact state. On the upper surface of the casing 11 on the upstream side, a raw material receiving port 111 for receiving the raw material from the quantitative feeder section 4 is opened. The spiral rod 12 is concentrically fixed to a drive shaft 121 of a drive motor (not shown) at the base end (right side in FIG. 1), and rotates about the shaft center via the drive shaft 121 by driving the drive motor. It is like that. A spiral fin 122 screwed in a predetermined direction is provided on the outer peripheral surface of the spiral rod 12, and the raw material supplied from the metering feeder unit 4 is sent to the kneading unit 2 by rotation around the axis of the spiral fin 122. It is designed to be pumped towards.

  The quantitative feeder unit 4 feeds a raw material to be continuously kneaded (in the present invention, a mixture of an organic pigment, a water-soluble inorganic salt and a water-soluble organic liquid, which is in the form of a sol or a gel). A raw material hopper 41 for containing the raw material, a spiral feeder 42 for feeding the raw material cut out from the bottom of the raw material hopper 41 toward the feed portion 1, and a downstream end of the spiral feeder 42 The casing 11 is provided with a connecting cylinder 43 standing from the peripheral edge of the raw material receiving port 111 so as to cover the casing 11.

  The spiral feeder 42 is mounted in a state in which a spiral fin is slidably contacted in an interposed cylinder 44 interposed between the bottom opening of the raw material hopper 41 and the upper opening of the connecting cylinder 43, and the proximal end side ( The right side in FIG. 1 is concentrically connected to a drive shaft of a feed motor (not shown). Therefore, the raw material in the raw material hopper 41 is conveyed by the spiral feeder 42 by rotating around the axis of the spiral feeder 42 driven by the feed motor, and is introduced into the casing 11 in advance via the interposed cylinder 44 and the connecting cylinder 43. It is designed to be supplied with a set conveyance amount.

  The kneading section 2 includes a plurality of fixed disks 21, annular kneading cylinders 22 arranged alternately with the fixed disks 21 while being sandwiched between the fixed disks 21, front and back surfaces (the left and right surfaces in FIG. 1). ) Is provided with a rotating disk 23 concentrically inserted into the kneading cylinder 22 in a state of facing the fixed disk 21. A tie rod (not shown) is passed through the plurality of fixed disks 21 and kneading cylinders 22, and a base end portion of the tie rods is fixed to the casing 11 of the feed portion 1, whereby the fixed disks 21 and the kneading cylinders 22 are fed. It is integrated with part 1.

Each of the rotating disks 23 is externally fitted on a spline shaft (not shown) that is concentrically provided from the distal end surface of the spiral rod 12. A cylindrical intermediate screw 24 is interposed between the adjacent rotating disks 23, so that the rotating disks 235 and the screws 24 are alternately mounted on the spline shaft. The rotating disk 23 has an outer diameter dimension set to be slightly smaller than the inner diameter dimension of the fixed disk 21, and the intermediate screw 24 has an outer diameter dimension set to be slightly smaller than the inner diameter dimension of the rotating disk 23. Each rotary disk 23 and each intermediate screw 24 are alternately fitted on the spline shaft, and the outer peripheral surface thereof passes through a gap through which the raw material can pass with respect to the inner peripheral surface of the kneading cylinder 22 and the fixed disk 21. They are designed to face each other.

  According to the configuration of the continuous kneader 10, the raw material loaded in the raw material hopper 41 is discharged from the bottom of the raw material hopper 41 by driving the spiral feeder 42, and is connected via the interposed cylinder 44 and the connecting cylinder 43. It is introduced into the casing 11 of the feed part 1. The raw material introduced into the casing 11 is sequentially conveyed toward the kneading unit 2 on the downstream side by the rotation of the spiral fins 122 by the driving rotation of the spiral rod 12.

  The raw material transported to the kneading unit 2 is first of all the outer peripheral surface of the intermediate screw 24 on the most upstream side (right side in FIG. 1) rotating around the axis and the drive shaft 121 on the most upstream side. 1 passes between the peripheral surface, and subsequently passes between the left side surface in FIG. 1 of the uppermost fixed disk 21 and the right side surface of the uppermost rotating disc 23 rotating around the axis, The raw material is kneaded when passing through these gaps. The kneading operation on the raw material is repeated in a plurality of stages for the amount of installation of the fixed disk 21, the kneading cylinder 22, the rotating disk 23, and the intermediate screw 24, whereby a plurality of components of the raw material (in the present invention, organic pigment, water-soluble A kneading process is performed on the inorganic salt and the water-soluble organic liquid). The product obtained by the completion of the kneading process is discharged to the outside through the gap between the outer peripheral surface of the rotating disk 23 on the most downstream side and the inner peripheral surface of the fixed disk 21, that is, the discharge unit 3.

  2 is a front view (viewed from the right side of FIG. 1) or a rear view (viewed from the left side of FIG. 1) showing an embodiment of a fixed disk and a rotating disk applied to the continuous kneader shown in FIG. (A) is a cavity fan-shaped fixed disk 21a, (b) is a cavity fan-shaped rotating disk 23b, (c) is a cavity chrysanthemum-shaped fixed disk 21c, and (d) is a cavity chrysanthemum mold. The rotating disks 23d and (e) show the cavity mortar-shaped fixed disk 21e, and (f) shows the cavity mortar-shaped rotating disk 23f, respectively.

  As shown in FIG. 2, the fixed disk 21 is provided with a loose fitting hole 211 for loosely fitting to the concentric intermediate screw 24, and the front and rear surfaces (front side and rear surface) of the fixed disk 21. A plurality of concave portions (cavities (crushing spaces) 212) having an equal pitch are provided in the circumferential direction that are recessed from the loose fitting holes 211 in the radial direction. On the other hand, the rotating disk 23 is provided with an outer fitting hole 231 for fitting in close contact with a spline shaft (not shown) formed concentrically, and on the front and rear surfaces of the rotating disk 23, A cavity (crushing space) 232 corresponding to the cavity 212 of the disk 21 is recessed. The cavity 232 of the rotating disk 23 is open at the periphery.

  Then, the raw material introduced into the gap between the fixed disk 21 and the rotating disk 23 is sequentially pushed into the cavities 212 and 232 by being pressed by the drive of the spiral rod 12, and in this state the rotating disk 23 is pivoted. By rotating around the center, a shearing force is applied to the raw material in each of the cavities 212 and 232 at the interface between the cavities 212 and 232. That is, the raw materials in the cavities 212 and 232 of the fixed disk 21 and the rotating disk 23 facing each other are sliced at the ridges of the ridges of the cavities 212 and 232, and the raw materials are replaced with shearing force (sheared raw materials). Are released from the cavities 212 and 232, and new raw materials enter the cavities 212 and 232), whereby the raw materials are kneaded and dispersed.

  The fixed disk 21 and the rotating disk 23 are formed into the cavity fan-shaped fixed disk 21a and the cavity fan-shaped rotating disk 23b shown in FIGS. 2 (a) and 2 (b) according to the shape of the cavities 212 and 232, and FIG. Cavity chrysanthemum type fixed disk 21c and cavity chrysanthemum type rotary disk 23d shown in (c) and FIG. 2 (d), cavity mortar type fixed disk 21e and mold shown in FIG. 2 (e) and FIG. 2 (f). The reason why it is divided into a plurality of types with the tee mortar type rotating disk 23f is to increase the shearing force on the raw material as the kneading and dispersing process proceeds.

  That is, the porosity of each cavity 212, 232 (the ratio (%) of the area of each cavity 212, 232 to the surface area of the fixed disk 21 and the rotating disk 23) is the fan-shaped cavities 212, 232, chrysanthemum. The mold cavities 212 and 232 and the mortar mold cavities 212 and 232 decrease in this order, but the shearing force on the raw material increases as the porosity decreases.

In the present embodiment, the cavities 212 and 232 have the fan-shaped fixed disk 21 and the rotation from the upstream side toward the downstream side in order to increase the shearing force on the raw material as the kneading and dispersing process proceeds on the raw material. The disk 23, the cavities 212, 232 are arranged in a chrysanthemum-shaped fixed disk 21 and the rotating disk 23, and the cavities 212, 232 are arranged in the mortar-shaped fixed disk 21 and the rotating disk 23 in this order.
By doing so, a large shearing force does not act on the raw material suddenly, but as the kneading and dispersing process proceeds, the shearing force on the raw material gradually increases. Thus, the organic pigment, the water-soluble inorganic salt, and the water-soluble organic liquid, which are constituents of the raw material, can be reliably mixed and dispersed with each other.

  Further, according to the continuous kneader 10 having such a configuration, when the organic pigment that is one of the constituent elements of the raw material is composed of coarse particles, the organic pigment is separated from the gap between the fixed disk 21 and the rotating disk 23 (particularly, By being introduced into each of the cavities 212 and 232), the organic pigment can be pulverized by applying a shearing force to the coarse particles by the rotation of the rotating disk 23.

  On the other hand, when the organic pigment is composed of agglomerates of fine particles, the agglomerates are introduced into the gaps (in particular, the respective cavities 212 and 232) between the stationary disk 21 and the rotating disk 23, so The aggregate can be reliably crushed and sized by rotation.

  Hereinafter, the pigment that is kneaded and dispersed by the continuous kneader 10 will be described in detail. The pigment of the present invention is concentric with the fixed disk 21 that rotates a mixture of an organic pigment, a water-soluble inorganic salt, and a water-soluble organic liquid around the axis of the annular fixed disk 21 and the drive shaft 121. It is obtained by kneading in a continuous kneader 10 having a pulverization space formed in a gap with the rotating disk 23.

  The organic pigment used in the present invention is one that can obtain finely sized particles by selecting appropriate reaction conditions at the time of synthesis, such as an azo pigment, and at the time of synthesis, such as a chlorinated copper phthalocyanine pigment. It means that the very fine and agglomerated particles produced are grown and sized in the subsequent process, and the coarse and irregular particles produced during synthesis such as copper phthalocyanine pigment are refined and sized in the subsequent process. Further, the pigment is not particularly limited as long as it is a pigment that requires refinement and sizing, and any conventionally known pigment can be used. For example, in addition to azo pigments, phthalocyanine pigments, and quinacridone pigments, isoindolinone, isoindoline, perylene, perinone, diketopyrrolopyrrole, thioindigo, dioxazine, quinophthalone, anthraquinone, and indanthrone can be used. Two or more kinds of pigments can be mixed and refined.

  The water-soluble inorganic salt used in the present invention is not particularly limited, and examples thereof include sodium chloride (sodium chloride), potassium chloride, sodium sulfate, zinc chloride, calcium chloride or a mixture thereof.

  As the water-soluble organic solvent used in the present invention, an organic pigment and a water-soluble inorganic salt are added so as to form a uniform mass, and are mixed freely with water, or are not mixed freely but are industrially washed with water. It is not particularly limited as long as the pigment particles grow, but the temperature rises at the time of kneading, and the solvent easily evaporates. preferable. For example, 2- (methoxymethoxy) ethanol, 2-butoxyethanol, 2- (isopentyloxy) ethanol, 2- (hexyloxy) ethanol, diethylene glycol, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monobutyl ether, triethylene glycol , Triethylene glycol monomethyl ether, liquid polyethylene glycol, 1-methoxy-2-propanol, 1-ethoxy-2-propanol, dipropylene glycol, dipropylene glycol monomethyl ether, dipropylene glycol monoethyl ether, low molecular weight polypropylene glycol, aniline , Pyridine, tetrahydrofuran, dioxane, methanol, ethanol, isopropyl Nol, n-propanol, isobutanol, n-butanol, ethylene glycol, propylene glycol, propylene glycol glycol monomethyl ether acetate, ethyl acetate, isopropyl acetate, acetone, methyl ethyl ketone, dimethylformamide, dimethyl sulfoxide, N-methylpyrrolidone, etc. Can do. Moreover, you may mix and use 2 or more types of solvents as needed.

  The amount of the water-soluble inorganic salt in the kneaded composition in the present invention is in the range of 7 to 30 times by weight of the water-soluble inorganic salt with respect to the organic pigment. When the water-soluble inorganic salt is less than 7 times by weight, it is difficult to make it finer, and when it exceeds 30 times by weight, it becomes possible to obtain a finer pigment, but since the amount of pigment processing decreases, productivity decreases. This is industrially disadvantageous. In other words, it can be produced by subjecting the organic pigment to solvent salt milling under a condition where the amount of the water-soluble inorganic salt used is larger than that of the conventional one.

  Further, the amount of the water-soluble organic liquid in the kneaded composition in the present invention is in the range of 0.3 to 7 times by weight of the water-soluble organic liquid with respect to the organic pigment, It can be selected according to the hardness of the kneaded composition. When the water-soluble organic liquid is less than 0.3 times by weight, the kneaded composition becomes too hard to be stably operated, and when it exceeds 7 times by weight, the kneaded composition becomes too soft and the fineness level is lowered.

  The operating conditions of the continuous kneader in the present invention are not particularly limited, but in order to control the throughput and the quality of the pigment, the mixing ratio of the kneaded composition, kneading temperature, mechanical energy input amount (main shaft (drive shaft 121) It is possible by adjusting the rotational speed, the amount of raw material supplied, the main shaft power load, and the like. Among them, the kneading temperature is 10 to 150 ° C., particularly 40 to 40 ° C. in order to effectively advance the organic pigment particle grinding and the organic pigment particle growth by contact with the water-soluble organic solvent. It is preferable that it is 130 degreeC. By increasing the temperature, it is possible to accelerate the growth rate of the pigment particles. On the other hand, by lowering the temperature, it is possible to suppress the growth of the pigment particles and further reduce the size. On the other hand, when the temperature is higher than 150 ° C., the particle growth is large and it is necessary to shorten the kneading time. It is also possible to change the growth of pigment particles by heating or cooling as necessary after the start of kneading and changing the kneading temperature for each machine zone.

  The organic pigment after kneading is treated by a conventional method. That is, the kneaded composition is treated with water or an aqueous mineral acid solution, and the organic pigment is isolated by removing the water-soluble inorganic salt and the water-soluble organic solvent by filtration and washing with water. The organic pigment can be used in a wet state as it is, or in a powder state by drying and grinding. If necessary, a resin, a surfactant and other additives may be added after kneading.

The use of the organic pigment produced by the method according to the present invention is not particularly limited, but it can be used for applications requiring high gloss and coloring power in addition to commonly used color materials. For example, when a gravure ink is prepared, the vehicle to be used is not particularly limited, and may contain an auxiliary agent or extender pigment. As one example, gravure ink vehicles include gum rosin, wood rosin, tall oil rosin, lime rosin, rosin ester, maleic acid resin, polyamide resin, vinyl resin, nitrocellulose, cellulose acetate, ethyl cellulose, chlorinated rubber, cyclized rubber, Ethylene-vinyl acetate copolymer resin, urethane resin, polyester resin, alkyd resin, acrylic resin, gilsonite, dammar, shellac, etc., or a mixture of the above resins or a water-soluble resin obtained by water-solubilizing the above resins, or an emulsion resin And hydrocarbons, alcohols, ketones, ether alcohols, ethers, esters, water, and the like. Particularly, cellulose-based materials with high gloss and clear quality can be obtained. In addition, when mixing or dispersing an organic pigment in a vehicle, good mixing or dispersion can be performed by using a dissolver, a high speed mixer, a homomixer, a kneader, a flasher, a roll mill, a sand mill, an attritor, or the like as a dispersing machine. it can.
Hereinafter, the present invention will be described in detail with reference to examples and comparative examples according to conventional methods. However, the present invention is not limited to the scope of these examples. In the examples, “parts” represents parts by weight, and “%” represents% by weight.

100 parts of crude copper phthalocyanine Blue 15 (T-95 Crude Blue manufactured by Zhuhai Toyo Co., Ltd.), 1000 parts of sodium chloride, and 150 parts of diethylene glycol were premixed for 5 minutes with a convert mixer (manufactured by Asada Tekko Co., Ltd.). This mixture is supplied to a continuous kneader 10 (“Miracle K.K.K.-42” manufactured by Asada Tekko Co., Ltd.) with a screw type quantitative feeder (quantitative feeder section 4 (FIG. 1)), and the crude pigment is ground. Thus, an organic pigment was produced. The conditions of the continuous kneading machine 10 are as follows: the feed part screw diameter is 120 mmφ, the number of kneading part sets is 8 consisting of a fixed disk and a rotating disk, the kneading composition is extruded at 22 kg / hour, the spindle speed is 50 rpm, and the kneading temperature is 100 ° C. Drove. The obtained kneaded composition was taken out to 10000 parts 1% aqueous solution of sulfuric acid 70 ° C., after 1 hour kept stirred, filtered, washed with water, dried ones are a specific surface area of ^90m 2 / g by BET method, TEM ( When observed with an electron microscope, all pigment particles were finely dispersed, and no coarse particles were observed. In addition, as a result of calculating the average diameter of the primary particle by image-analyzing the TEM photograph, it was 43 nm. Furthermore, compared with the pigment obtained by the manufacturing method of the comparative example 1 shown below, it refined | miniaturized more. In addition, the input amount of electric power energy per 1 kg of pigment was 3.1 kwh / kg, which was 44% of that of Comparative Example 1. In addition, 10 parts of the pigment composition, 90 parts of gravure ink varnish (nitrocellulose resin 12%, ethyl acetate 33%, toluene 30%, isopropyl alcohol 15%, methanol 10%) and 3 parts of 3 mm glass beads, The gravure ink prepared by dispersing for 60 minutes with a paint conditioner was spread on a film with a bar coater and the 60 ° gloss value was measured to be 84%.

[Comparative Example 1]
100 parts of crude copper phthalocyanine Blue15 (T-95 Crude Blue, manufactured by Zhuhai Toyo Co., Ltd.), 1000 parts of sodium chloride, and 150 parts of diethylene glycol are charged into a 1000-capacity part double-arm kneader to form a dense lump at 100 to 110 ° C. While holding, the mixture was kneaded for 5 hours. After grinding, it was taken out to 10000 parts of a 1% aqueous sulfuric acid solution at 70 ° C., stirred for 1 hour with heat, filtered, washed with water and dried to obtain a copper phthalocyanine pigment. This had a specific surface area of 73 m ² / g by the BET method, and the image analysis value of the TEM photograph measured in the same manner as in Example 1 was 64 nm. The amount of power energy input per 1 kg of pigment was 7.1 kwh / kg. Further, the gloss value of the developed color product produced in the same manner as in Example 1 was 68%.

100 parts of crude copper phthalocyanine Blue 15 (T-95 Crude Blue manufactured by Zhuhai Toyo Co., Ltd.), 2000 parts of sodium chloride, and 230 parts of diethylene glycol were premixed for 5 minutes with a convert mixer (manufactured by Asada Tekko Co., Ltd.). This mixture is supplied to a continuous kneader 10 (“Miracle K.K.K.-42” manufactured by Asada Tekko Co., Ltd.) with a screw type quantitative feeder (quantitative feeder section 4 (FIG. 1)), and the crude pigment is ground. Thus, an organic pigment was produced. The conditions of the continuous kneader 10 are as follows: the feed part screw diameter is 120 mmφ, the number of kneading part sets is 8 consisting of a fixed disk and a rotating disk, the extrusion rate of the kneaded composition is 23 kg / hour, the spindle speed is 50 rpm, and the kneading temperature is 60 ° C. Drove. The kneaded composition obtained here was taken out in 20000 parts of a 1% aqueous sulfuric acid solution at 70 ° C., heated and stirred for 1 hour, filtered, washed with water, and dried, which had a specific surface area of 107 m ² / g by the BET method, When observed with an electron microscope, all pigment particles were finely dispersed, and no coarse particles were observed. In addition, as a result of calculating the average diameter of the primary particle by image-analyzing the TEM photograph, it was 35 nm. Furthermore, compared with the pigment obtained with the manufacturing method of the comparative example 2 shown below, it refined | miniaturized more. In addition, the input amount of electric power energy per 1 kg of pigment was 6.5 kwh / kg, which was 32% of Comparative Example 2. In addition, the gloss value of the developed color product produced in the same manner as in Example 1 was 87%.

“Comparative Example 2”
100 parts of crude copper phthalocyanine Blue 15 (T-95 Crude Blue manufactured by Zhuhai Toyo Co., Ltd.), 2000 parts of sodium chloride, and 230 parts of diethylene glycol were charged into a 1000-capacity part double-arm kneader to form a dense lump at 65 to 75 ° C. While holding, the mixture was kneaded for 7 hours. After grinding, it was taken out in 20000 parts of a 1% aqueous sulfuric acid solution at 70 ° C., stirred for 1 hour with heat, filtered, washed with water and dried to obtain a copper phthalocyanine pigment. This had a specific surface area of 88 m ² / g by BET method, and the image analysis value of a TEM photograph measured in the same manner as in Example 1 was 45 nm. The amount of power energy input per 1 kg of pigment was 20.2 kwh / kg. Further, the gloss value of the color developed product prepared in the same manner as in Example 1 was 83%.

“Comparative Example 3”
100 parts of crude copper phthalocyanine Blue 15 (T-95 Crude Blue manufactured by Zhuhai Toyo Co., Ltd.), 400 parts of sodium chloride, and 70 parts of diethylene glycol were premixed for 5 minutes with a convert mixer (manufactured by Asada Tekko Co., Ltd.). This mixture is supplied to a continuous kneader 10 (“Miracle K.K.K.-42” manufactured by Asada Tekko Co., Ltd.) with a screw type quantitative feeder (quantitative feeder section 4 (FIG. 1)), and the crude pigment is ground. Thus, an organic pigment was produced. The conditions of the continuous kneader 10 are as follows: the feed part screw diameter is 120 mmφ, the number of kneading part sets is 8 consisting of a fixed disk and a rotating disk, the extrusion rate of the kneaded composition is 20 kg / hour, the spindle speed is 50 rpm, and the kneading temperature is 60 ° C. Drove. The kneaded composition obtained here was taken out into 20000 parts of a 1% aqueous sulfuric acid solution at 70 ° C., heated and stirred for 1 hour, filtered, washed with water, and dried, which had a specific surface area of 78 m ² / g by the BET method, When observed with an electron microscope, all pigment particles were finely dispersed, and no coarse particles were observed. In addition, as a result of calculating the average diameter of the primary particle by image-analyzing the TEM photograph, it was 52 nm. The amount of power energy input per 1 kg of pigment was 1.2 kwh / kg. In addition, the gloss value of the color developed product produced in the same manner as in Example 1 was 73%.

Crude dioxazine violet Violet 23 (Sumitomo Chemical Co., Ltd., Sumitone First Violet RL base) 100 parts of pigment, 2000 parts of sodium chloride, and 210 parts of diethylene glycol were mixed in the same continuous kneader 10 as in Example 1 and the extrusion rate of the kneaded composition was 20 kg / hour. The organic pigment was obtained by operating at a spindle speed of 50 rpm and a kneading temperature of 90 ° C. The pigment content in the obtained kneaded product was purified, filtered and dried in the same manner as in Example 1. As a result, the specific surface area was 101 m ² / g, and TEM observation showed that all pigment particles were finely dispersed. Coarse particles were not observed. In addition, as a result of calculating the average diameter of the primary particle by image-analyzing the TEM photograph, it was 37 nm. Furthermore, compared with the pigment obtained with the manufacturing method of the comparative example 4 shown below, it refined | miniaturized more. Further, the input amount of electric power energy per 1 kg of pigment was 6.3 kwh / kg, which was 32% of that of Comparative Example 4. In addition, the gloss value of the color developed product produced in the same manner as in Example 1 was 87%.

“Comparative Example 4”
Crude dioxazine violet Violet 23 (Sumiton First Violet RL base manufactured by Sumitomo Chemical Co., Ltd.) 100 parts of pigment, 2000 parts of sodium chloride, and 100 parts of diethylene glycol were charged into a 1000-volume part double-arm kneader and dense lump at 90-95 ° C ( The mixture was kneaded for 7 hours while maintaining the dough). After grinding, it was taken out in 20000 parts of a 1% aqueous sulfuric acid solution at 70 ° C., held and stirred for 1 hour, filtered, washed with water and dried to obtain a dioxazine violet pigment. This had a specific surface area of 87 m ² / g by the BET method, and the image analysis value of a TEM photograph measured in the same manner as in Example 1 was 41 nm. The amount of power energy input per kg of pigment was 19.8 kwh / kg. Further, the gloss value of the color developed product produced in the same manner as in Example 1 was 82%.
The production conditions in each example and the performance of the obtained pigment are shown in Table 1.

It is sectional drawing of the side view which shows one Embodiment of the continuous kneading machine which concerns on this invention. FIG. 2 is a front view or a rear view showing one embodiment of a fixed disk and a rotating disk applied to the continuous kneader shown in FIG. 1, (a) is a cavity fan type fixed disk, and (b) is a cavity fan type rotation. (C) is a cavity chrysanthemum fixed disk, (d) is a cavity chrysanthemum rotary disk, (e) is a cavity mortar fixed disk, and (f) is a cavity mortar rotary disk. .

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 Continuous kneading machine 1 Feed part 11 Casing 111 Raw material receiving port 12 Spiral rod 121 Drive shaft 122 Spiral fin 2 Kneading part 21 Fixed disk 21a Cavity fan type fixed disk 21c Cavity chrysanthemum type fixed disk 21e Cavity mortar type fixed disk 211 Free fitting hole 212 Cavity (grinding space)
22 Kneading cylinder 23 Rotating disk 23b Cavity fan type rotating disk 23d Cavity chrysanthemum type rotating disk 23f Cavity mortar type rotating disk 231 External fitting hole 232 Cavity (grinding space)
DESCRIPTION OF SYMBOLS 3 Discharge part 4 Fixed_quantity | feed_rate feeder part 41 Raw material hopper 42 Spiral feeder 43 Connection cylinder 44 Interposition cylinder

Claims (2)

A mixture of an organic pigment, a water-soluble inorganic salt of 7 to 30 times by weight with respect to the organic pigment, and a water-soluble organic liquid of 0.3 to 7 times by weight with respect to the organic pigment And a continuous kneader having a pulverization space formed in a gap portion between the fixed disk and the fixed disk rotating integrally around the axis of the drive shaft and a concentric rotating disk. Method. The method for producing a pigment according to claim 1, wherein the kneading temperature is controlled to 10 to 150 ° C.

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