JP2990212B2 - Colored resin composition and method for producing the same - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention is applicable to uses other than image recording.
Regarding the method for producing the pigment resin composition to be used , more specifically, it is used for purposes other than image recording excellent in dispersibility of the pigment.
The purpose of the present invention is to provide a colored resin composition.

[0002]

2. Description of the Related Art Conventionally, pigment resin compositions, for example, as a colorant for plastics, a dry color in which a pigment is mixed with a dispersant, a master batch in which a pigment is kneaded with a carrier resin at a high concentration, and the like have been widely used. These colorants for plastics disperse the pigment by melting and kneading the pigment powder and a dispersant or a carrier resin with a high shearing machine such as a roll or a kneader. Since there are many agglomerated particles, all these coarse particles are several μm
It is very difficult to redistribute to: In the coloring of conventional plastics, it is preferable that the presence of coarse particles is, of course, preferred, but fine dispersion was not so strictly required.

[0003]

On the other hand, in recent years, high dispersibility of pigments has been strongly required even in coloring of plastics and fibers, and the conventional method using powdered pigments is not suitable. Is becoming more difficult .

[0004] As a method of obtaining a pigment resin colored material having excellent dispersibility, an aqueous paste of a pigment and a resin are kneaded to transfer an aqueous pigment to a resin phase, and then water is removed to remove the pigment. However, a method for producing a resin composition has been proposed (see Japanese Patent Application Laid-Open No. 2-175770). However, in this method, the presence of a pigment paste is assumed, and the pigment as a raw material can be obtained only as a powder pigment. If not, it cannot be applied. In addition, in such a method, a large amount of water contained in the pigment paste to be used requires a step of drainage and evaporation, and the energy consumption thereof cannot be neglected. Accordingly, an object of the present invention is to provide a pigment resin composition in which a pigment is finely dispersed at a high concentration without using an aqueous paste of the pigment, for example, a colorant useful for resins, fibers, and other uses, and the colorant. to provide a <br/> colored resin composition that is used for applications other than for image recording that has been colored by.

[0005]

The above object is achieved by the present invention described below. That is, the present invention is not limited to image recording.
In a pigment resin composition in which a pigment is finely dispersed in a resin, a dry pigment, a hot-melt resin and water as a dispersing agent are charged into a mixer or kneader and mixed. and the resin was wet, was heated and kneaded by melting the resin by heating under pressure or normal pressure, moisture normally圧或colored resin composition, wherein the benzalkonium be dried removed by evaporation under reduced pressure And a method of manufacturing the same.

[0006]

According to the present invention as described above, by adding water as a dispersing agent and kneading the pigment and the resin under pressure or at normal pressure, the movement of water molecules becomes active and the powder pigment It is considered that water permeates into the higher order aggregates of the above, breaks down the aggregates, and is dispersed and diffused in the resin in a state of lower order aggregate particles close to the time of pigment synthesis. Accordingly, firstly, the effect of the dispersion is that the effect of dispersing the pigment is much improved compared to the ordinary dry kneading method, and the fine particles of the pigment which cannot be obtained by mechanical dispersion can be dispersed. Secondly, it is sufficient to add an appropriate amount of water necessary for dispersion, as described later. Therefore, when the pigment and the resin are removed after kneading, it is only necessary to evaporate under heating or reduced pressure.

Third, the addition of water improves the releasability between the melt and the metal part of the kneader, and the melt expands due to the vapor pressure of water, whereby uniform dispersion proceeds smoothly. Fourth,
In the case of kneading at normal pressure, the temperature rise due to frictional heat of kneading can be suppressed by using the latent heat of evaporation of water, and kneading for a long time is possible by adding more water.
More complete dispersion of the pigment can be achieved. or,
The colorant composition thus obtained is further added to the intended use resin, if necessary, and the mixture is diluted and kneaded to obtain a colored resin composition having excellent dispersibility of the pigment and a clear practical pigment concentration. I can do it.

[0008]

Next, the present invention will be described more specifically with reference to preferred embodiments. As the pigment used in the present invention, conventionally known chromatic and black to white organic pigments and inorganic pigments are used. For example, azo series, polycondensed azo series, azo series containing azomethine group, azomethine series, anthraquinone Pigments, phthalocyanine-based, perinone-perylene-based, indigo-thioindigo-based, dioxazine-based, quinacridone-based, isoindolinone-based, aniline black-based pigments and iron oxide-based spinel structures, carbon black-based pigments, titanium oxide-based pigments and the like. No. Among them, organic pigments having particularly high lipophilicity are preferred.

As the resin used in the present invention, any of conventionally known thermoplastic resins and resins used as carrier resins for masterbatches can be used.
Further, when a high-concentration colorant is prepared, a carrier resin of a master batch which is compatible with the colorant can be used.
For example, polystyrene, styrene- (meth) acrylate copolymer, styrene-maleate copolymer, rosin-modified maleic resin, (meth) acrylate polymer and copolymer, styrene-diene copolymer Coalesce, polyethylene resin, polypropylene resin, polyester resin, epoxy resin, petroleum resin, alkyd resin, polyvinyl chloride resin, polyvinylidene chloride resin, acrylonitrile styrene resin, ethylene vinyl acetate resin, polycarbonate resin, acetal resin, Polyamide resins and various waxes are used.

Preferred among the above resins are resins which have a melting point or softening point of about 150 ° C. or lower, and are preferably solid at room temperature of 130 ° C. or lower. The ratio between the pigment and the resin component varies depending on the purpose of the colored resin composition, and is about 20 to 70% by weight in the case of a high-concentration composition. 0.01 to 10% by weight
It is.

As the water used in the present invention, ion-exchanged water, drinking water, distilled water, steam, industrial water and the like are used. The amount of water added is 1 to the total weight of the dry pigment and the resin.
２００200% by weight, preferably 5-100% by weight.
The method of the present invention is how you heat melting <br/> A charge pressure or normal pressure kneader and such dry pigment and hot-melt resin and water mentioned above. Since the kneading in the kneading machine is performed in a state where the resin is molten, the kneading is performed at a temperature of about 70 to 130 ° C.

At the time of production, a powder pigment, a hot-melt resin and water are mixed in advance with a Hensyl mixer or the like, and the mixture is charged into a flasher, kneader, extruder, roll mill, or the like. The water-soluble resin and water are charged and mixed. Then heated under pressure or normal pressure to melt the resin by kneading and dispersing, followed by removal of water remaining was dried by atmospheric pressure or evaporated under reduced pressure, the pigment resin kneaded product are obtained. Then, it is further added to the resin to be colored for use and diluted and kneaded to produce a clear and clear colored resin with good dispersion.

[0013]

Next, the present invention will be described more specifically with reference to examples. In the description, parts or% are based on weight. Example 1 100 parts of AC polyethylene 6A (manufactured by Allied Chemical & Die Corporation) and stable copper phthalocyanine blue powder pigment (CI Pigment Blue 15: 3) 60
And 80 parts of ion-exchanged water were charged into a kneader-type kneader, mixed for 10 minutes, and the resin fine powder and the powder pigment were wetted with ion-exchanged water and heated gradually as it was. Almost 95-11
The resin is melted at 0 ° C, kneaded in a state where water is mixed, and kneaded at 95 to 110 ° C for 20 minutes while evaporating water.
The temperature was raised to 20 ° C., and the kneading was continued to evaporate the remaining water, followed by dehydration and drying. Kneading was further continued at 120 to 130 ° C. for 10 minutes.

After cooling, the mixture is further kneaded with three heated rolls.
After cooling and crushing, a high-concentration colored resin composition containing a blue pigment at a concentration of 30% was obtained. This was placed on a slide glass, heated and melted, and observed under a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed. One part of the above composition and 100 parts of polyethylene (Sumikasen G-201, manufactured by Sumitomo Chemical Co., Ltd.) were kneaded with an extruder to obtain a sharply colored resin. When this was observed with a microscope by the same method, all the pigment particles were finely dispersed, and no coarse particles were recognized.

Example 2 Epoxy resin (Epicoat 1004, manufactured by Shell Sekiyu KK)
100 parts of powdered pigment and 80 parts of carmine 6B (CI Pigment Red 57: 1) and ion-exchanged water 11
0 parts were charged into a kneader-type kneader, mixed for 10 minutes, and the resin fine powder and the powder pigment were wetted with ion-exchanged water and gradually heated as it was. The resin melts at about 95-110 ° C,
The mixture was kneaded in a state where water was mixed, and the mixture was kneaded at 95 to 110 ° C. for 20 minutes while evaporating the water. Then, the temperature was raised to 120 ° C., and the kneading was continued to evaporate the remaining moisture and dehydrate and dry.

The kneading was further continued at 120 to 130 ° C. for 10 minutes. After cooling, the mixture was further kneaded with a heating three rolls, cooled and crushed to obtain a high-concentration colored resin composition containing a blue pigment at a concentration of 30%. This was placed on a slide glass, heated and melted, and observed under a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed. One part of the above composition and 100 parts of the epoxy resin were mixed together in a powder extruder and kneaded with an extruder to obtain a sharply colored resin. This was placed on a slide glass, heated and melted, and observed with a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed.

Example 3 Methyl methacrylate resin (manufactured by Sanyo Chemical Industries, Hymer S)
BM600) and 100 parts of a polycondensed azo pigment (C.I.
Pigment Yellow 128) 70 parts of the powdery dry pigment and 100 parts of ion-exchanged water are charged into a kneader-type kneader.
After mixing for 1 minute, the resin fine powder and the powder pigment were wetted with ion-exchanged water and gradually heated. About 95-110 ° C
The resin is melted and kneaded in a state where water is mixed, and the mixture is kneaded at 95 to 110 ° C. for 20 minutes while evaporating water, and then 120 ° C.
The mixture was further kneaded to continue the kneading, evaporating the remaining water and dehydrating and drying. Kneading was further continued at 120 to 130 ° C. for 10 minutes.

After cooling, the mixture is further kneaded with three heated rolls.
After cooling and crushing, a high-concentration colored resin composition containing a blue pigment at a concentration of 30% was obtained. This was placed on a slide glass, heated and melted, and observed under a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed. 1 part of the above composition and methyl methacrylate resin 100
After mixing the powder, the mixture was kneaded with an extruder to obtain a sharply colored resin. This was placed on a slide glass, heated and melted, and observed with a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed.

Example 4 Polyester Resin (Ket R247, manufactured by Toray Industries, Inc.) 100
And 90 parts of water and 90 parts of dimethylquinacridone (CI Pigment Red 57: 1) were charged into a kneader-type kneader and mixed for 10 minutes, and the resin fine powder and the powder pigment were wetted with ion-exchanged water. And gradually heated. The resin melts at about 90 to 100 ° C, and is kneaded in a state where water is mixed, and the water is evaporated for 90 minutes to 90 to 90 ° C.
After kneading at 0 ° C., the temperature was raised to 120 ° C., and the kneading was continued to evaporate the remaining water, followed by dehydration and drying.

Kneading was further continued at 120 to 130 ° C. for 10 minutes. After cooling, the mixture was further kneaded with a heating three rolls, cooled and crushed to obtain a high-concentration colored resin composition containing a blue pigment at a concentration of 30%. This was placed on a slide glass, heated and melted, and observed under a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed. One part of the above composition and 100 parts of a polyester resin were mixed with a powder and kneaded with an extruder to obtain a sharply colored resin. This was placed on a slide glass, heated and melted, and observed with a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed.

Example 5 Polystyrene resin (manufactured by Sanyo Chemical Co., Ltd., Hymer ST-9)
5) 100 parts and stable copper phthalocyanine blue pigment 6
0 parts of the powder pigment and 80 parts of water were charged into a kneader type kneader and mixed for 10 minutes, and the resin fine powder and the powder pigment were wetted with ion-exchanged water and heated gradually as it was. Almost 90-1
The resin is melted at 00 ° C., kneaded in a state where water is mixed, and kneaded at 90-100 ° C. for 20 minutes while evaporating water.
The temperature was raised to 20 ° C., and the kneading was continued to evaporate the remaining water, followed by dehydration and drying. Kneading was further continued at 120 to 130 ° C. for 10 minutes. After cooling, the mixture was further kneaded with a heating three rolls, cooled and crushed to obtain a high-concentration colored resin composition containing a blue pigment at a concentration of 30%. This was placed on a slide glass, heated and melted, and observed under a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed.

One part of the above composition and polystyrene resin 100
After mixing the powder, the mixture was kneaded with an extruder to obtain a sharply colored resin. This was placed on a slide glass, heated and melted, and observed with a microscope. As a result, all the pigment particles were finely dispersed, and no coarse particles were observed.

[0023]

According to the present invention as described above, the following effects can be expected by adding water as a dispersing aid and kneading under pressure or under normal pressure. First, the dispersing effect is much improved as compared with the ordinary dry kneading method, and fine particle dispersion that cannot be obtained by mechanical dispersion can be achieved. Second, the amount of water to be used is sufficient by adding an appropriate amount necessary for dispersion.
Therefore, when it is removed after kneading, it is only necessary to evaporate under heating or reduced pressure.

Third, the releasability between the melt and the metal part of the kneader is improved by the addition of water, the melt expands due to the vapor pressure of water, and uniform dispersion proceeds smoothly. Fourth, when kneading at normal pressure, the temperature rise due to frictional heat of kneading can be suppressed by utilizing the latent heat of evaporation of water,
Further, by adding water, kneading can be performed for a long time, and the pigment can be more completely dispersed. Further, the colorant composition thus obtained is further added to a resin for use as needed, and the mixture is diluted and kneaded to obtain a colored resin composition having excellent dispersibility and a clear practical pigment concentration. I can do it.

──────────────────────────────────────────────────続 き Continuing on the front page (72) Michie Nakamura 1-7-6 Nihombashi Bakurocho, Chuo-ku, Tokyo Inside Dainichi Seika Kogyo Co., Ltd. (72) Yoshimasa Nakamura 1-chome Nihonbashi Bakurocho, Chuo-ku, Tokyo No. 7 in Dainichi Seika Kogyo Co., Ltd. (72) Inventor Jusuji Hamada 1-7-6 Nihonbashi Bakurocho, Chuo-ku, Tokyo In Dainichi Seika Kogyo Co., Ltd. (56) References JP-A-53-88844 (JP) JP-A-3-47710 (JP, A) JP-A-6-148937 (JP, A) (58) Fields investigated (Int. Cl. ⁶ , DB name) B29B 7/88

Claims (7)

(57) [Claims] 1. A pigment resin composition in which a pigment is finely dispersed in a resin, which is used for purposes other than image recording .
A dry pigment, a hot-melt resin and water as a dispersing agent are charged and mixed in a mixer or kneader to wet the pigment and the resin, and then heated under pressure or normal pressure to melt the resin and heat-knead. after, moisture normally圧或colored resin composition characterized and Turkey be dried removed by evaporation under reduced pressure. 2. The colored resin composition according to claim 1, wherein the pigment is a chromatic, black or white organic pigment and / or an inorganic pigment. 3. The colored resin composition according to claim 1, wherein the water content is 1 to 200 parts by weight based on 100 parts by weight of the total amount of the pigment and the resin. 4. The colored resin composition according to claim 1, wherein the colored resin composition is a solid composition containing a pigment at a high concentration. 5. A colored resin composition obtained by adding the colored resin composition according to claim 1 to a resin to be colored and diluting and kneading it. 6. Coloring used for purposes other than image recording
In the production of a resin composition, a dry pigment and a hot-melt resin and water as a dispersing aid are mixed in a mixer or kneader, mixed and wetted, and the pigment and the resin are wetted and heated under pressure or under normal pressure. after by melting the resin by heating and kneading a pigment and a resin Te, moisture normally圧或the method for producing a colored resin composition, wherein the dry removal to Turkey <br/> evaporated under reduced pressure. 7. A method for producing a colored resin composition, comprising adding the colored resin composition according to claim 6 to a resin to be colored and diluting and kneading the resin.