JPH11286555A - Production of granular colorant and production apparatus therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a granular colorant having suppressed reaggregation and excellent pigment dispersibility, by soft blending and heat granulation in a low-speed revolving container by gravity without a conventional forced stirring type heat granulation using a Henschel mixer or the like. SOLUTION: A granular thermally meltable substance as a carrier is melted, pigment particles are attached to the melted substance by dispersion or included dispersedly and granulated by using a granulating apparatus in which a container main body capable of controlling a temperature is rotated at a low speed, and a container supporting body 3 is subjected to at least one additional movement of rotation, rocking and reciprocation so that the pigment is not reaggregated to give the objective granular colorant having excellent dispersibility. The granular colorant is guided to a heat blending apparatus, heated, blended and granulated by a granular to give a granular colorant having more excellent dispersibility.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] The present invention relates to a method for producing a granular colorant. In detail, a method of producing a granular colorant by a production apparatus in which a container body capable of controlling the temperature inside is rotated, and a support of the container performs at least one additional motion of rotation, swinging, and reciprocating motion. . That is, this method is a method of gradually heating the container or the inside thereof, melting the hot-melt carrier material to adhere the pigment, further fusing the hot-melt materials together, dispersing and containing the pigment, and obtaining a particulate colorant. .
The coloring agent obtained in the present invention has a low movement of the container and is heated and granulated while stirring and mixing softly, so that the pigment is not re-agglomerated, and the pigment is included in the hot-melt carrier material. Therefore, even when a coloring agent molded product is obtained by adding to a molding resin, the pigment does not re-aggregate, so that a colored molded product in which the pigment is sufficiently dispersed can be obtained.

The colorant obtained by the present invention is easy to handle because of its low scattering property and little equipment contamination, and also has good fluidity and automatic measuring property. And a master batch colorant having better pigment dispersibility can be obtained. This colorant can be used in molding applications requiring high pigment dispersibility, such as films and sheets.

[0003]

2. Description of the Related Art Colorants for resins generally include dry color in powder form, liquid color in liquid form, and master batch in pellet form.

[0004] Dry color is obtained by adding a dispersant such as a thermoplastic resin or metal soap to a pigment and mixing and dispersing the pigment. Although it has a high pigment content and is relatively inexpensive, it is in a powdery form and has poor workability during handling, that is, there are problems such as severe equipment contamination and lack of automatic weighing properties. Further, the pigment dispersibility is also poor.

[0005] In order to reduce the device contamination of the dry color and enhance the automatic weighing property, it is necessary to make the shape of the colorant granular. Generally, a hot-melt substance such as a thermoplastic resin or wax having a melting point and a softening point of 60 to 160 ° C. and a pigment are stirred in a vessel such as a Henschel mixer while the hot-melt substance is melted by frictional heat or forced heating. There is a granular bead colorant in which a pigment is adhered to the surface and the hot-melt substances are also fused together. Since this manufacturing method is also relatively simple, it is described in "Granulation Handbook", edited by Japan Powder Industry Association (issued in 1976), Chapter 9, "Agitated Granulation Method", and has many application examples. However, the molten carrier material adheres firmly to the inner wall of a container such as a Henschel mixer, it takes time to clean after removing the colorant, and the pigment is re-agglomerated due to forced stirring and mixing, resulting in poor pigment dispersibility. There are drawbacks such as not good. To solve these problems, Japanese Patent Publication No. Sho 56-398
Various improvements have been made to the process and the composition as in 21.
As a result, the granulation work becomes complicated, or the dispersant added for the purpose of improving dispersibility is easily transferred to the surface of the final molded product,
There are many problems such as lack of versatility of the colorant.

[0006] Liquid color has good dispersibility and automatic weighing property, but lacks versatility due to the use of a liquid surfactant and other dispersants, and is therefore less versatile than dry color and masterbatch colorants. Not much use.

[0007] The masterbatch colorant is prepared by adding a pigment, a thermoplastic resin, and, if necessary, a wax and an antistatic agent.
It is obtained by kneading with a single-screw extruder or a twin-screw extruder, dispersing the pigment, and granulating with a shaping machine. Since the pigment is in powder form and the thermoplastic resin is generally in pellet form, it is necessary to devise a method of supplying the extruder to the extruder. Generally, they are separately supplied to an extruder or mixed and supplied using a tumble mixer or Henschel mixer, but in any case, it is difficult to always supply the extruder uniformly with the pigment and the thermoplastic resin. . Therefore, the obtained colorant may cause color fluctuation in a lot, and thus the colorant is often kneaded once again with an extruder to stabilize the color. However, the colorant has good workability during molding use and relatively good pigment dispersibility.

Further, in order to obtain a highly dispersed masterbatch colorant, the pigment and the hot-melt carrier substance are pre-kneaded with a pressure kneader, a Banbury mixer, or the like, and then a twin-screw extruder or a three-roll heating machine. In many cases, a method for preparing a base having a high dispersion and a high pigment content by kneading the mixture and then kneading the base with a thermoplastic resin to form a master batch colorant has been adopted. According to this manufacturing method, the manufacturing process is complicated, so that the delivery date is long and the price is high.

[0009]

DISCLOSURE OF THE INVENTION The present invention is a method for obtaining a granular colorant having improved pigment dispersibility, which has improved drawbacks of dry color and bead color. Rather than the conventional forced stirring type granulation using a Henschel mixer, etc., granulation is performed while heating and mixing softly by gravity in a low-speed rotating container to suppress pigment reagglomeration. It is a method of obtaining an agent. This colorant is easy to handle,
Since it has good automatic weighing properties, it can always be easily supplied to a molding machine.

[0010] The present invention also enables the masterbatch to have a short delivery time and a low price. Since the colorant of the present invention is easy to handle and has good automatic weighing properties, it can always be uniformly supplied to the heating and kneading apparatus. In a single-screw extruder or a twin-screw extruder, the dispersibility and the color stability can be further improved by a single kneading. A good masterbatch colorant can be obtained.

[0011]

Means for Solving the Problems The inventors of the present invention have conducted intensive studies in view of such a situation, and as a result, have invented a method of obtaining a granular colorant for a thermoplastic resin having good pigment dispersibility.

That is, the present invention provides a method for producing a granular colorant in which pigment particles are dispersed and contained in a carrier containing a hot-melt substance. A container body capable of controlling the temperature inside the container body, the container body rotating around a first axis and rotating or swinging about a second axis, or at least one additional movement of reciprocating movement; Doing, using a stirrer that produces a stirring action of the contents by the action of the motion and gravity, while controlling the stirring so that the pigment does not re-agglomerate, until both are integrated into a granular form in the container body This method is characterized in that a pigment is dispersed and attached to a carrier by stirring, or a pigment is formed in a granular form while the pigment is dispersed and contained in the carrier to obtain a granular colorant.

[0013] The present invention also relates to an apparatus for carrying out such a method, comprising a container body capable of controlling the temperature inside, the container being provided with a rotation about a first axis.
Providing a drive for imparting at least one additional motion of rotation or rocking about a second axis, or reciprocating motion, thereby agitating the container contents under the action of multi-axial combined motion and gravity. The present invention relates to an apparatus for producing a granular colorant, comprising a stirrer that produces an action.

As a method of controlling the temperature inside the container of the manufacturing apparatus, the container body is heated from its outer surface and the contents of the container are heated through the vessel wall, or a heater is inserted into the container.
There is a method of heating the contents of the container by blowing hot air.

The granular colorant obtained above is introduced into a heating kneading apparatus such as a three-roll heating roll, a pressure kneader, a single-screw extruder, or a twin-screw extruder, and is heated and kneaded. The present invention relates to a production method characterized in that a granular colorant is obtained by guiding and granulating.

[0016]

DETAILED DESCRIPTION OF THE INVENTION Briefly describing the method and apparatus of the present invention, the temperature controllable container body rotates and the container support performs at least one additional motion of rotation, rocking and reciprocating motion. In a granulator, 0.1 to 99% by weight of the powdery pigment and 1 to 99.9% by weight of the powdery and granular hot-melt carrier material are placed in a container,
The container and the container support are moved, heat is further applied to the surface of the container or the inside of the container to melt the hot-melt carrier material, the pigment is dispersed and adhered to the surface, and the hot-melt materials are also adhered to each other to disperse and contain the pigment. A method of obtaining a granular colorant, and adding a thermoplastic resin or other additives to the colorant or this colorant if necessary, kneading with a heating kneading apparatus,
This is a method of obtaining a master batch colorant by dispersing a pigment more highly.

The specific components and conditions that can be selected in carrying out the present invention are described below. The thermoplastic resin to be subjected to the color molding of the colorant in the present invention, polyethylene resin, polypropylene resin, polyvinyl chloride resin, polyvinylidene chloride resin, polystyrene resin, acrylic resin, vinyl acetate resin, polyamide resin, polyethylene terephthalate resin, A homopolymer such as a polycarbonate resin, or a copolymer such as an acrylonitrile-butadiene-styrene resin or an ethylene-vinyl chloride resin, or a thermoplastic elastomer, or a thermoplastic composite material obtained by combining a glass fiber and a thermoplastic resin, etc. is there. When the coloring agent is added to these resins to form a colored molded product, the amount of the coloring agent to be added is 0.1 to 40% by weight, preferably 0.5 to 10% by weight in terms of a pure pigment.

The pigments include organic pigments, inorganic pigments, extender pigments, and metal powders. Organic pigments include, for example, azo-based pigments such as azo lake, insoluble azo, and condensed azo; phthalocyanine-based pigments such as phthalocyanine blue and phthalocyanine green; anthraquinone;
There are perylene and pigments such as perylene and perylene, and condensed polycyclic pigments such as quinacridone, isoindolinone, and dioxazine. Inorganic pigments include, for example, titanium pigments such as titanium oxide and titanium yellow, red iron oxide pigments such as iron oxide, yellow iron oxide, chromate pigments such as graphite and chromium vermillion, and aluminate pigments such as cobalt blue. Salt pigments, carbon black, and the like. In addition, the extender pigments include calcium carbonate, aluminum silicate, silica sand, calcium hydroxide, talc, clay, and mica.
Examples of the metal powder include brass powder and aluminum powder. The present invention is particularly effective when a colorant is formed using an organic pigment which is generally said to be difficult to disperse.

The carrier contains one or more types of hot-melt substances described below, and preferably is not limited in its content and type as long as it is in powder form, and may be composed of only hot-melt substances.
From the melting point and softening point of the hot-melt substance, group A is as follows:
When classified into Group B and used properly, preferable granules are easily obtained. For example, group A has a melting point and softening point of 10
There are thermoplastic resins such as polyethylene resin, polypropylene resin, polyvinyl chloride resin, polystyrene resin, and ABS resin, which are relatively high at 0 to 300 ° C. and have high melt viscosity. In addition, the melting point and softening point of Group B are 40 to 150.
℃ and relatively low polyethylene wax, polypropylene wax, low molecular weight thermoplastic resins such as polystyrene wax and their modified products, or montan wax, wax such as microcrystalline wax and their derivatives, or fatty acids such as stearic acid, oleic acid and Examples include fatty acid compounds such as calcium stearate and stearic acid amide, and surfactants such as polyoxyethylene polyoxypropylene block polymer and fatty acid sorbitan ester. As the hot-melt substance, one or more of either the group A or the group B, or one or more of the groups A and B are used in combination. The heat-melt substance of the group B having a relatively low melting point and softening point is used. Since the heating temperature is lower when is used, the thermal efficiency is better. Also,
The heat-melted substance of group A is used as a simple carrier,
It is effective when used in combination with a group of hot-melt substances. That is, in the case of the group B heat-melting substance alone, there is a danger of overheating and the whole being fused to form a rice cake. Is possible.

Although the melting point and softening point of the hot-melt material are known from literatures, books and manufacturer's instructions, the measuring methods are different from each other, so that all hot-melt materials cannot be compared with each other. The melting point and softening point of the present invention are not strictly defined because the melting point and softening point may not be clearly shown for some substances. In addition, since the surface of a hot-melt substance exhibits properties close to a molten state when heated at a temperature lower than the melting point and softening point, granulation proceeds even at a temperature lower than the melting point and softening point.

The shape of the hot-melt substance is preferably powdery or granular. Since thermoplastic resins are generally in the form of pellets,
It is preferable to select a brand that can be obtained in a powder form or a granular form of about 1 mm or less, or to crush the pellets into a powder form or a granular form with a crusher. Granulation is difficult when the total amount of the hot-melt substance is in the form of pellets, and in the case where the hot-melt substance is a combination of pellets and granules, after the granulation, a non-uniform colorant containing a mixture of pellets and grains Becomes However, even non-uniform colorants can be homogenized by kneading them with a heating kneading device such as a pressure kneader, a single screw extruder or a twin screw extruder and then shaping them into granules with a shaping device.

As a similar granulation method, there is a method in which a binder solution is sprayed into a granulator so that powders adhere to each other. If the hot-melt substance is melted in advance and sprayed from a nozzle inserted into the container, it is not impossible to use the granulator of the present invention to softly granulate as in the present invention. However, most of the commonly used hot-melt substances have a high melting point and softening point of 70 ° C. or higher, or have a high viscosity at the time of melting, so that it is difficult to spray in a mist state and sufficient granulation results can be obtained. hard.

The apparatus for producing a granular colorant in the present invention comprises:
Depending on the contents of the rotating container performing the additional motion, it can be classified into a rotary granulator, an oscillating granulator and the like. The rotary granulator is composed of a vertical double container, and the outer container and the inner container are connected by a bottom container shaft. The inner container rotates around the container axis, and the outer container rotates vertically around the support shaft at the center of the side surface while the inner container is contained. Temperature control is performed by supplying hot air, hot water, steam, or the like between the outer and inner containers (jacket) from a temperature control pipe. As such a granulating apparatus, for example, Japanese Utility Model Publication No. 5-9067 describes an apparatus for uniformly performing thermal processing of a granular material. In the oscillating granulator, a horizontal drum container rotates on a support, and the support oscillates like a seesaw around a central horizontal axis. The temperature is controlled by an electric heater or the like which is inserted into the container and does not directly contact the container wall. As such a granulating device, for example, Japanese Utility Model Publication No. Hei 6-11089 describes a device for granulating by adhering powder while melting a binder. In addition, as a method of controlling the temperature of the oscillating granulator, external heating such as mounting an infrared heater or the like inside a heat retaining cover that does not directly contact the rotating container to heat the outer surface of the container, inserting a heater inside the container, and applying hot air There is a method of internal heating that heats the air. To perform heating quickly, external heating is effective, and internal heating is preferably used supplementarily.

The additional movement of the container and the container support of the granulator is performed at a relatively low speed. Generally, the rotation speed of the container is 50 rpm or less, and the rotation speed or swing frequency of the container support is 30 rpm or 30 revolutions per minute, respectively. The movement speed differs depending on the capacity of the container, the kind of the contents and the melting point and the softening point, but at least the rotation speed of the container is 30.
rpm or less is preferable. Number of rotations of stirring blades of a forced stirring type granulator such as Henschel mixer is 1000 to 200.
Compared with 0 rpm, the moving speed for stirring and mixing of this granulator is very low, indicating that the granulation can be performed softly while suppressing the re-aggregation of the pigment.

The granulation time is dominated by the melting point and softening point of the hot-melt substance, but is also influenced by the type and amount of the pigment, or the heating and kinetic conditions of the granulator. Set temperature to 10
It is 40 to 60 minutes when the temperature is set to 0 ° C. In a forced stirring type granulator, granulation can be carried out at 20 to 40, but granulation proceeds rapidly after melting the hot melt substance. Therefore, if the stop of stirring is delayed, there is a high risk that the material will be caked.

A heating kneader for kneading the granular colorant to further improve the dispersibility includes a pressure kneader, a Banbury mixer, a three-roll heater, a single screw extruder, a special single screw extruder, and a twin screw extruder. And its usage is not particularly limited.

The present invention is a method for producing a granular colorant having good dispersibility using the above-mentioned materials and a granulating apparatus.
The details are described below. 0.1-99% by weight of pigment powder,
A material containing preferably 10 to 80% by weight and 1 to 99% by weight, preferably 5 to 80% by weight of the hot-melt substance granules as a carrier is put in a container, and the container rotates and the support rotates and shakes. Motion or at least one additional motion of reciprocating motion. Further, the temperature of the contents is gradually increased by heating the container with a heater or a jacket, and when the temperature reaches a preset temperature near the melting point and the softening point, the heating is stopped. The hot-melt material gradually melts near the set temperature, causes the pigment to adhere to the surface thereof, and the hot-melt materials also adhere to each other, contains the pigment, and is completely granulated after reaching the set temperature. The content temperature further rises within 5 ° C. due to residual heat even after the heating is stopped, but thereafter gradually decreases. In order to sufficiently perform granulation, the set temperature should be close to the melting point and softening point of the hot-melt substance.
When the hot-melt substance is contained in an amount equal to or higher than the oil absorption of the pigment, the content may be formed into a rice cake when heated to a temperature higher than its melting point and softening point. Therefore, when raising the temperature of the content above the melting point and softening point of the hot-melt substance, it is preferable to make the hot-melt substance less than the oil absorption of the pigment.

When two or more heat-melting substances having different melting points and softening points, preferably different by 10 ° C. or more, are used in combination, a coloring agent having less fear of sticking and having large grains can be obtained. For example, 50% by weight of a pigment is added with 25% by weight of each of two types of hot-melt substances having different melting points and softening points of Group A and Group B by 10 ° C. or more, and the set temperature is set between the melting point and the softening point of both the melting points. It is good to granulate as temperature.

[0029]

EXAMPLES The present invention will be specifically described below with reference to examples and comparative examples, but the present invention is not limited thereto. In the examples, parts and% are based on weight.

Example 1 Fastgen Green S, each in powder form
(Phthalocyanine pigment, manufactured by Dainippon Ink and Chemicals) 50
Part, high wax NL800 (low molecular weight polyethylene,
49 parts of softening point 111 ° C., manufactured by Mitsui Petrochemical Co., Ltd.) and 1 part of zinc stearate (manufactured by Seido Chemical Co., Ltd., melting point: 120 ° C.) are put in a rotary granulator, and the rotation speed of the container is 30 rpm, and the rotation of the support shaft is performed. Operation was performed at several 15 rpm, and hot water at 120 ° C. was passed through the jacket and heated. The heating was stopped when the temperature of the contents in the container gradually rose to the set temperature of 80 ° C. Thereafter, the operation was continued after stopping the flow of the hot water, and after 10 minutes, the cooling water was passed. When the temperature of the contents was cooled to 60 ° C., the operation was stopped and taken out to obtain a granular colorant. 10 parts of this coloring agent and 90 parts of low-density polyethylene were rolled at 120 ° C.
The mixture was diluted and kneaded with two heated rolls having a roll clearance of 0.5 mm for 2 minutes and then taken out into a sheet having a thickness of 0.3 mm. Approximately 10 samples each from any five locations on this sheet
mg was cut out, sandwiched between two glass plates, the sample was rolled by a press at 200 ° C., and observed with a microscope of 100 times. The pigment coarse particles in each sample were measured, and the maximum particle size therein was determined, which was used as the evaluation value of the pigment dispersibility. Also,
0.4 part of this colorant, 3 parts of a master batch of 60% titanium oxide, and 96.6 parts of low-density polyethylene are kneaded with white by kneading with two heated rolls having a roll clearance of 0.5 mm and then put into a cooling press. The sheet was 2 mm thick.
Using a color difference meter CS-5 chroma sensor, the wavelength is 610 nm.
, And k / s, which is the ratio between the absorption k and the reflectance s, was determined. Next, the raw pigment Fas was used instead of 0.4 part of the colorant.
Using 0.2 parts of tgen GreenS and 0.2 parts of low density polyethylene, a sheet was prepared in the same manner and k / s
I asked. The tinting power of this colorant is the k / s of the raw pigment.
Is a standard (100), and is represented by a comparative value of k / s of the colorant. Table 1 shows the evaluation results.

Example 2 A slightly larger granular colorant was obtained in exactly the same manner as in Example 1, except that the temperature was set to 100 ° C. instead of 80 ° C. The pigment dispersibility and coloring power of this colorant were determined in the same manner. Next, after raising the temperature of the contents to 110 ° C., which was higher than in the same manner as in Example 1, heating was stopped, but the test was interrupted because the contents began to solidify into a rice cake during the cooling operation.

Example 3 The colorant obtained in Example 1 was heated at a roll temperature of 120 ° C.
Knead with this roll (manufactured by Inoue Mfg. Co., Ltd.), thickness 2-3mm
Sheet. This sheet was brittle at normal temperature, and after coarse crushing, it was put into a funnel pressure equipped with a 5 mm screen and pulverized to obtain a granular colorant having a thickness of 1 to 3 mm and a length of 2 to 4 mm. The pigment dispersibility and coloring power of this colorant were determined in the same manner as in Example 1. Table 1 shows the evaluation results.

Example 4 The colorant obtained in Example 2 was kneaded with a heated three rolls to obtain a granular colorant in the same manner as in Example 3. Next, the pigment dispersibility and coloring power of this colorant were determined in the same manner as in Example 1. Table 1 shows the evaluation results.

Comparative Example 1 25 parts of a powdery dry color (Dylene Color K-5, pigment content 20%, manufactured by Dainippon Ink and Chemicals, Inc.) composed of powdery Fastgen Green S and metal soap, respectively, and low density polyethylene 75 Was diluted and kneaded in the same manner as in Example 1 to determine the pigment dispersibility. Also,
1 part of this dry color, 3 parts of a 60% titanium oxide masterbatch and 96 parts of low-density polyethylene were kneaded with white in the same manner as in Example 1, and the coloring power was determined. Table 1 shows the evaluation results.

Comparative Example 2 The same compounding material as in Example 1 was placed in a 20 L Henschel mixer (manufactured by Mitsui Mining Co., Ltd.) and stirred at 1000 rpm.
When stirring was continued while heating by passing steam through the jacket, the resistance applied to the stirring shaft increased when the content temperature exceeded 90 ° C., and the ammeter rapidly increased from 10 amps to 20 amps. Transfer the contents to a cooling mixer for 30 minutes.
The mixture was cooled and stirred at 0 rpm and taken out when the temperature of the content became 60 ° C. or lower to obtain a granular colorant. The pigment dispersibility and coloring power of this colorant were determined in the same manner as in Example 1. Table 1 shows the evaluation results.

Comparative Example 3 The colorant obtained in Comparative Example 2 was kneaded in the same manner as in Example 3 to obtain a granular colorant. The pigment dispersibility and coloring power of this colorant were determined in the same manner as in Example 1. Table 1 shows the evaluation results.

Comparative Example 4 The same compounding material as in Example 1 was mixed with a Henschel mixer and kneaded with a heated three rolls as in Comparative Example 3 without granulation. Even though three parallel rolls were closely adhered to each other and the rolls were squeezed so that there was no gap, the pigment could spill out from between the rolls, or the high wax NL800 was fused to the rolls and kneading could not be performed. The test was interrupted. Pigment scattering was also intense, and the area around the heated three rolls was stained with pigment.

Example 5 Sandorin Red BN each in powder form
(Condensed azo pigment, manufactured by Sando Co., Ltd.) 30 parts, sun wax 1
61P (low molecular weight polyethylene, softening point 111 ° C., manufactured by Sanyo Chemical Co., Ltd.) 20 parts, Tokuyama Polypro PN240A
(Polypropylene, softening point 150 ° C, manufactured by Tokuyama Soda Co., Ltd.)
50 parts are put into the oscillating granulator, and the rotation speed of the container is 30 rpm.
m, the support was rotated at a frequency of 22 times / minute, and the surface of the container was heated by an infrared heater on the inner surface of the heat retaining cover that did not directly contact the container. When the surface temperature reached 150 ° C., the temperature was maintained. The temperature of the contents in the container also gradually rises,
When the temperature reached 10 ° C., the heating was stopped. Thereafter, the heater was stopped and the operation was continued, and the operation was stopped after the content temperature was cooled to 80 ° C., and the heater was taken out to obtain a granular colorant. This was kneaded with a twin-screw extruder PCM-30 (manufactured by Ikegai Iron Works) at a set temperature of 170 ° C. and a screw rotation speed of 400 rpm to obtain a pellet colorant. After mixing 16.7 parts of this coloring agent and 83.3 parts of Tokuyama Polypropylene PN240A (polypropylene, manufactured by Tokuyama Soda Co., Ltd.), the pigment dispersibility was determined in the same manner as in Example 1. Table 2 shows the evaluation results.

Comparative Example 5 The same compounding material as in Example 5 was prepared in the same manner as in Comparative Example 2.
A granulated colorant is obtained by stirring granulation, and this is a twin-screw extruder PC
The mixture was kneaded with M-30 to obtain a pellet colorant. With respect to this colorant, the pigment dispersibility was determined in the same manner as in Example 1. Table 2 shows the evaluation results.

Comparative Example 6 The same formulation as in Example 5 except that Tokuyama Polypro MS240 (polypropylene, softening point 150 ° C., manufactured by Tokuyama Soda Co., Ltd.) made of the same resin and pellets was used instead of the powdery Tokuyama Polypro PN240A. The materials were kneaded with a twin-screw extruder PCM-30 just by mixing with a Henschel mixer to obtain a pellet-shaped colorant. When sampling from five places of this colorant, there were a dark part and a light part. Then, the colorant was put in a tumbler and mixed well, and then kneaded again with PCM-30 to obtain a pellet-shaped colorant. With respect to this colorant, the pigment dispersibility was determined in the same manner as in Example 1. Table 2 shows the evaluation results.

Example 6 Each of 95 parts of powdered Toda red handle 120ED (ferric oxide, manufactured by Toda Kogyo KK) and 95 parts of zinc stearate (melting point: 120
5 ° C, manufactured by Shodo Chemical Co., Ltd.)
The container was operated at a rotation speed of the container of 30 rpm and the number of times of swing of the support base was 22 times / min. The temperature of the contents in the container was also gradually increased, but since the temperature reached 120 ° C., the heating was stopped. Since then
The heater was stopped and operated, and the content was cooled to 80 ° C., so the operation was stopped and taken out to obtain a granular colorant. 2.1 parts of this coloring agent and Dick Styrene CR-3500
(General-purpose polystyrene, manufactured by Dainippon Ink and Chemicals, Inc.) 9
After mixing 7.9 parts, a card size plate was made with a 1 oz in-line injection molding machine. Approximately 10 mg of each sample was cut out from any five places on this plate, and thereafter the pigment dispersibility was determined in the same manner as in Example 1. Table 3 shows the evaluation results.

Comparative Example 7 A coloring agent was obtained in exactly the same manner as in Example 6, except that the stirring and mixing operation was carried out at room temperature for 20 minutes without heating the content to 120 ° C. However, the contents were slightly granulated, but the equipment contamination was severe. Next, the pigment dispersibility was determined in the same manner as in Example 6. Table 3 shows the evaluation results.

Comparative Example 8 The same compounding material as in Example 6 was placed in a vertical mixing and stirring apparatus (Henschel mixer, manufactured by Mitsui Mining Co., Ltd.), and a granular colorant with less scattering was obtained in the same manner as in Comparative Example 2. Next, the pigment dispersibility was determined in the same manner as in Example 6. Table 3 shows the evaluation results.

[0044]

According to the present invention, since the pigment and the hot-melt substance are heat-granulated while being softly mixed, the pigment does not re-aggregate and a granular colorant having good dispersibility can be obtained. In addition, since this coloring agent has little scattering and contamination properties and has good automatic measuring properties, it can be easily introduced into a heating kneading apparatus, and can be a coloring agent having good pigment dispersibility.

[0045]

[Table 1] Coloring power: The relative value of the k / s of each colorant when the k / s of the raw pigment is set to 100 as a standard is expressed as the coloring power.

[0046]

[Table 2]

[0047]

[Table 3]

[Brief description of the drawings]

FIG. 1 is an elevational view conceptually showing one example of a rotary granulator according to the present invention.

FIG. 2 is an elevational view conceptually showing one example of an oscillating granulator according to the present invention.

[Explanation of symbols]

 In FIG. 1, 1 outer container 2 inner container 3 support shaft 4 temperature control pipe 5 pedestal 6 container shaft 7 lid 1 in FIG. 6 Fixed pedestal 7 Support center axis 8 Lid

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁶ Identification code FI B29B 9/10 B29B 9/10 C08J 3/20 C08J 3/20 C // B01J 2/12 B01J 2/12 B29K 101: 12 C08L 101: 00

Claims (5)

[Claims] 1. A method for producing a granular colorant in which pigment particles are dispersed and contained in a carrier containing a hot-melt substance, wherein the inside of the hot-melt substance powder and the pigment powder are temperature-controlled. Wherein the container body rotates about a first axis and performs at least one additional motion of rotation, or rocking, or reciprocating motion about a second axis, the motion of And a stirrer that produces a stirring action of the contents by the action of gravity, while controlling the stirring so that re-aggregation of the pigment does not occur, while stirring the two until they are integrated into the container body. A method for producing a granular colorant, comprising dispersing and attaching a pigment to a carrier, or shaping into a granule while dispersing and incorporating the pigment in the carrier. 2. The container according to claim 1, wherein the container body is heated from its outer surface and the contents of the container are heated through the vessel wall, or the contents of the container are heated by inserting a heater inside the container or blowing hot air. Method. 3. A method for producing a granular colorant, comprising: introducing the granular colorant obtained in claim 1 or 2 into a heating and kneading apparatus, heating and kneading the same, and then introducing the same into a granulator and granulating it. 4. The heating kneading apparatus is a three-roll heating roll, a pressure kneader, a single screw extruder, a twin screw extruder, or the like.
The method described in. 5. A container body capable of controlling the temperature inside the container body,
The container is provided with a drive for providing at least one additional movement of rotation or swinging about a second axis, or reciprocating movement, together with rotation about a first axis, whereby a multi-axis composite is provided. An apparatus for producing a granular colorant, comprising a stirrer that generates a stirring action on the contents of a container by the action of motion and gravity.