JPH09131727A - Device for manufacturing master batch of coloring agent - Google Patents

Abstract

PROBLEM TO BE SOLVED: To obtain a high kneading ability and various kneading characteristics matching with a resin material or blending agent by providing a two stripe kneading disc at the part corresponding to the melting and kneading part of a screw, and also providing flow passage control means for a resin flow passage between the melting and kneading part and an extrusion part. SOLUTION: A resin flow passage is controlled by flow passage control means comprising a torpedo ring 7 and slide valve 8 disposed at the downstream side from a melting and kneading part C corresponding to the sort of resin material or sort of a blending agent to be kneaded in resin. As a result, molten resin stays within the melting and kneading part C during the specified period of time, and resin pressure is intensified up to a given pressure. In addition, by an interaction with a plurality of grooves 3 formed in a third cylinder block 2c and a kneading disc 6, i.e., a shearing effect and extension effect caused by the kneading disc 6, and a positional replacing effect and resin flow divisional effect or the like caused by the repeated coming in and out movement of each groove 3, effective melting and kneading are executed with the consequence that the blending agent is dispersed finely and uniformly.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a colorant masterbatch manufacturing apparatus for manufacturing a colorant masterbatch in which a colorant is finely and uniformly dispersed.

[0002]

2. Description of the Related Art Conventionally, in order to produce a colorant masterbatch in which a pigment such as titanium dioxide or carbon black is finely and uniformly dispersed in a polyolefin resin such as polyethylene or polypropylene, a batch type Banbury mixer or an intensive mixer is used. Instead of the above, a single-screw extruder or a twin-screw extruder having a kneading disk, a mixing pin, a kneading element such as a barrier flight, or the like capable of continuous operation is used.

[0003]

However, among the above-mentioned conventional techniques, a single-screw extruder having a kneading element cannot increase the shear rate and the shear stress, and therefore the high quality limit extrusion amount can be increased. It is not possible, and the production volume per unit time is low.

On the other hand, a twin-screw extruder having a kneading element can increase the shear rate and shear stress by setting the screw rotation speed higher than that of the above-mentioned single-screw extruder, so that the extrusion amount per unit time is large. Although it increases to some extent, the kneading characteristics of the kneading element are fixed at the time of designing.Therefore, various kneading characteristics suitable for the kind of resin material and the kind of pigment kneaded in the resin material, that is, the kind of compounding agent are required. There was a problem that it could not be obtained and lacked versatility.

The present invention has been made in view of the problems of the above-mentioned conventional techniques, and has high kneading performance and can obtain various kneading characteristics suitable for the types of resin materials and compounding agents. The purpose is to realize a manufacturing apparatus for a colorant masterbatch.

[0006]

In order to achieve the above object, a manufacturing apparatus for a colorant masterbatch according to the present invention comprises a cylinder and two meshing type screws rotatably arranged in the cylinder. In a manufacturing apparatus for a colorant masterbatch having at least a transport section, a melting / kneading section, and an extruding section, a plurality of recesses are formed at intervals on the inner wall surface of the cylinder corresponding to the melting / kneading section. And at least two kneading discs are provided at a portion of the screw corresponding to the melting / kneading portion,
A flow path adjusting means for adjusting the opening of the resin flow path in the cylinder is provided between the melting / kneading section and the extruding section.

The plurality of recesses may be formed of a plurality of axially extending grooves formed at intervals in the circumferential direction of the cylinder, or a plurality of recesses formed at intervals. Can be.

Further, the flow path adjusting means is composed of a torpedo ring formed on the screw and at least two slide valves which can move forward and backward with respect to the torpedo ring, and the slide valves are spaced from each other in the circumferential direction of the cylinder. It is effective if they are arranged at intervals.

[0009]

The resin material and the compounding agent supplied to the transportation section are conveyed to the melting / kneading section, and in the melting / kneading section, a plurality of recesses provided on the inner wall surface of the cylinder and at least two screws provided on the screw are provided. Due to the interaction of the strip kneading disks, they are melted and kneaded by being subjected to shearing action, extension action, position exchange action, flow dividing action, etc., and the compounding agent is finely and uniformly dispersed in the molten resin. In addition, by adjusting the opening degree of the resin flow path formed between the screw and the inner wall surface of the cylinder by the flow path adjusting means, the flow of the resin is retained for a predetermined time so that the resin pressure in the melting / kneading part is controlled. By raising the pressure to a predetermined level, it is possible to obtain melting / kneading characteristics corresponding to the type of compounding agent.

In the present invention, examples of the resin material used include polyolefin resins such as homopolymers of ethylene and α-olefins such as propylene and copolymers of at least two kinds of the above olefins. Particularly preferred polyolefin resins are low, medium and high density polyethylene resins and polypropylene resins. The molecular weight of the polyolefin resin is not particularly limited, but is usually 10,000.
At 100,000, the MI value is 2-70.

The range of pigments and additives used as compounding agents is as inorganic pigments such as titanium oxide, rouge, ultramarine, complex oxides, carbon black, etc., and as organic pigments, cyanine blue, cyanine. Green type, quinacridone type, polyazo type, monoazo type, perylene type, perinone type, hindered phenol,
As an ultraviolet absorber such as thioether and phosphite,
Examples of light stabilizers such as benzophenone and triazole include hindered amines. For example, the additive is preferably in the range of 0.1 to 0.3% by weight with respect to 100 parts of the resin. Furthermore, as the fatty acid metal salt that can be used in the present invention, magnesium stearate, calcium stearate, aluminum stearate, zinc stearate, lithium stearate, and the like can be used, and the pigment can be used in an amount of 0.
The range of 05 to 5% by weight is preferable.

[0012]

DESCRIPTION OF THE PREFERRED EMBODIMENTS One embodiment of the present invention will be described with reference to the drawings.

As shown in FIGS. 1 to 3, a colorant masterbatch manufacturing apparatus 1 of this embodiment includes a cylinder 2 composed of cylinder blocks 2a to 2f connected to each other,
It has two meshing type screws 4 each rotatably arranged in the cylinder 2 and a rotation driving means (not shown) for rotating both screws 4 in the same direction, and it is provided from the upstream side to the downstream side. Sequential supply section A and solid transport section B
From the melt-kneading part C, the slot part D in which the flow path adjusting means for adjusting the opening of the resin flow path in the cylinder 2 is arranged, the degassing part E and the melt-transporting part F. It is equipped with an extrusion section.

The supply section A is composed of a first cylinder block 2a having a supply port 10 and a full flight section 5 of a screw 4, and a solid transportation section B is adjacent to the downstream side of the first cylinder block 2a. It is composed of a second cylinder block 2b and a full flight portion 5 of the screw 4.

The melting / kneading section C includes a third cylinder block 2c adjacent to the downstream side of the second cylinder block 2b,
It is composed of at least two kneading discs 6 provided on the screw 4, and a plurality of recesses are formed on the inner wall surface of the third cylinder block 2c as shown in FIG. A plurality of grooves 3 extending in the direction are formed at intervals in the circumferential direction in the cross section perpendicular to the axis.

On the downstream side of the third cylinder block 2c,
A fourth cylinder block 2d is connected to the fourth cylinder block 2d, and the torpedo ring 7 provided on the screw 4 and the fourth cylinder block 2d are slidable from each other in the circumferential direction in a cross section perpendicular to the axis. A flow path adjusting means including at least two slide valves 8 movably provided and capable of advancing and retracting with respect to the torpedo ring 7 is provided, and each slide valve 8 is driven by a driving means such as a fluid pressure cylinder (not shown). By advancing / retreating with respect to the torpedo ring 7, the opening degree of the resin flow path 9 formed in the cylinder 2 can be adjusted.

Downstream of the fourth cylinder block 2d,
A fifth cylinder block 2e having a vent port 11 and a sixth cylinder block 2f are sequentially connected, and a full flight part 5 is formed at a portion of the screw 4 corresponding to the fifth cylinder block 2e and the sixth cylinder block 2f. ing. In addition, a cap 1 is attached to the tip of the screw 4.
2 are installed.

The cylinder 2 does not necessarily have a plurality of cylinder blocks 2a, 2b ..., 2f as in this embodiment.
However, if the cylinder 2 having a plurality of cylinder blocks 2a, 2b, ..., 2f connected thereto is used as in this embodiment, the processing is easy.

Next, the operation of this embodiment will be described.

The resin material and the compounding agent supplied from the supply port 10 are sequentially conveyed to the melting / kneading section C via the supply section A and the solid transport section B, and during this period, the cylinder 2 is heated by a heating means (not shown). The temperature rises due to heat transfer from and heat generated by shearing. In the melting / kneading section C, the groove 3
By the interaction between the kneading disk 6 and the kneading disk 6, the compounding agent is finely and uniformly dispersed in the molten resin.

The kneading action in the melting / kneading section C will be described in more detail. According to the kind of resin material and the kind of compounding agent kneaded in the resin, the kneading operation is provided on the downstream side of the melting / kneading section C. Torpedo ring 7 and slide valve 8
The opening degree of the resin flow path is adjusted by the flow path adjusting means. As a result, the molten resin stays in the melting / kneading section C for a predetermined time, and the resin pressure is increased to a predetermined pressure. In addition, the plurality of grooves 3 formed in the third cylinder block 2c
And interaction with the rotating kneading disc 6,
That is, the kneading disk 6 effectively performs the melting and kneading due to the shearing action and the extending action, the position exchange action due to the repeated entry and exit of each groove 3, the dividing action of the resin flow, and the like, and the compounding agent is finely mixed in the molten resin. And evenly dispersed.

The molten resin material in which the compounding agent is finely and uniformly dispersed in the melting / kneading section C is degassed of volatile components through the vent port 11 in the degassing section E,
The melt is transported to the melt transport section F and extruded from a die (not shown).

The plurality of recesses provided in the portion corresponding to the melting / kneading portion C on the inner wall surface of the cylinder 2 are not limited to the groove 3 described above, and a plurality of depressions such as hemispheres or semi-flat spheres may be formed on each other. It may be arranged randomly or regularly at intervals.

The two screws 4 can be rotated in opposite directions, and instead of the slide valve 8, a rod-shaped body or a plate-shaped body which can advance and retreat in the radial direction in the cross section perpendicular to the axis of the cylinder 2 can be used. can do.

In order to confirm the effect of the present invention, a comparative experiment was conducted between the specific example of the present invention and the comparative example. The results will be described below.

(Specific Example 1) Kneading extruder used: A meshing type co-rotating twin-screw kneading extruder having a cylinder bore of 69 mm and L / D = 42.5 similar to the above-mentioned embodiment (manufactured by Japan Steel Works Ltd.) TEX65α-42.5AW-2V) Operating conditions: Extrusion rate 500 kg / hour, screw rotation speed 400 rpm Cylinder temperature: Room temperature in supply part, 50-100 ° C in kneading part, 120-180 ° C in extruding part Compounding agent: Titanium dioxide ( DuPont R101) 60 parts, antioxidant (Ciba Geigy, Irganox B225) 0.2 parts Zinc stearate 3 parts, low density polyethylene (density 0.920.MFR5) 40 parts premixed with a Henschel mixer. What I did. The above compounding ingredients were weighed using a Brabender weighing machine and fed from a feed port to produce a masterbatch for paper laminating.

(Specific Example 2) Kneading extruder used: Same as specific example 1 Operating conditions: Same as specific example 1 Cylinder temperature: room temperature in supply part, 140-165 ° C in kneading part, 140-200 ° C in extruding part Compounding agent: Titanium dioxide (Dupont, R101) 60 parts, antioxidant (Ciba Geigy, Irganox 1010) 0.2 parts Magnesium stearate 3 parts, polypropylene (density 0.921, MFR26) 40 parts Premixed with an oil mixer.

The above compounding ingredients were supplied in the same manner as in the specific example to produce a masterbatch for paper laminating.

(Specific Example 3) Kneading extruder used: Same as specific example 1 Operating condition: Same as specific example 1 Cylinder temperature: Same as specific example 1 Compounding agent: Rouge (Bayer, Bayferrox 130M) 60 parts Antioxidant (manufactured by Ciba Geigy, Irganox B225) 0.2 parts Zinc stearate 3 parts and low density polyethylene (density 0.916, MFR26) 40 parts premixed with a henschel mixer.

The above compounding ingredients were supplied in the same manner as in Example 1 to produce a masterbatch for film.

(Specific Example 4) Kneading extruder used: Same as specific example 1 Operating conditions: Same as specific example 1 Cylinder temperature: Same as specific example 1 Compounding agent: Ultramarine blue (Daiichi Kasei Co., Ltd., # 1500) 60 parts, antioxidant (Ciba Geigy, Irganox B225) 0.2 parts Zinc stearate 3 parts, low density polyethylene (density 0.916, MI26) 40 parts premixed with a Henschel mixer.

The above compounding ingredients were supplied in the same manner as in Example 1 to produce a masterbatch for film.

(Example 5) Kneading extruder used: Same as example 1 Operating conditions: Same as example 1 Cylinder temperature: Same as example 1 Compounding agent: Carbon black (Carbon Black # 30 manufactured by Mitsubishi Kasei Co., Ltd.) ) 30 parts Antioxidant (Yoshitomi Pharmaceutical Co., Ltd., Yoshinox SR) 0.2 part, low density polyethylene (density 0.920, MI7) 70 parts premixed with a Henschel mixer.

The above compounding ingredients were fed in the same manner as in Example 1 to produce a masterbatch for pipes.

(Specific Example 6) Kneading extruder used: same as in Example 1 Operating conditions: same as in Example 1 Cylinder temperature: same as in Example 1 Compounding agent: carbon black (manufactured by Cabot Co., Vulcan 9-32A) 30 parts Antioxidant (Yoshitomi Pharmaceutical Co., Ltd., Yoshinox SR) 0.2 parts, low density polyethylene (density 0.916, MI26) premixed with a Henschel mixer.

The above compounding ingredients were supplied in the same manner as in Example 1 to produce a masterbatch for pipes.

(Comparative Example 1) Instead of the twin-screw kneading extruder,
Example 1 using a 50 liter Banbury mixer
80% filling volume of Banbury mixer
In the above, heating and water cooling were controlled so that the maximum temperature did not exceed 160 ° C., and mixing was performed for 15 minutes to produce a masterbatch for lamination.

(Comparative Example 2) Using a 50 liter Banbury mixer, the same mixture as in Example 2 was mixed for 15 minutes by controlling heating and water cooling so that the maximum temperature did not exceed 180 ° C, and laminating. Masterbatch for.

Comparative Example 3 Using a 50-liter Banbury mixer, the same mixture as in Example 3 was mixed for 15 minutes by controlling heating and water cooling so that the maximum temperature did not exceed 160 ° C., and the film was mixed. Masterbatch for.

(Comparative Example 4) Kneading extruder used: An interlocking type co-rotating twin-screw kneading extruder having a conventional structure and having no means for adjusting grooves and flow paths in the melting / kneading section (cylinder bore diameter 69 mm, L / D = 42.5) Operating conditions: Extrusion rate 400 to 450 kg / hour, Screw rotation speed 400 rpm Cylinder temperature: Same as in Example 1 Compounding agent: Same as in Example 4, master batches for films were produced under the above conditions.

Comparative Example 5 Using a 50 liter Banbury mixer, the same ingredients as in Example 5 were mixed for 15 minutes by controlling heating and water cooling so that the maximum temperature did not exceed 160 ° C. A masterbatch for pipe was manufactured.

(Comparative Example 6) Kneading extruder used: Same as Comparative Example 4 Operating conditions: Same as Comparative Example 4 Cylinder temperature: Same as Example 1 Compounding agent: Same as Example 6 Master for pipe under the above conditions A batch was produced.

Table 1 shows the results of the evaluation of the coloring power, the film dispersion, and the pressure increase ΔP of the master batches produced by the above-mentioned specific examples and comparative examples.

Here, the coloring power, the film dispersion, and the pressure increase ΔP will be briefly described.

Coloring power The following reference materials (1), (2) and (3) are prepared. TiO ₂ = titanium oxide, LDPE = high-pressure polyethylene, PP = polypropylene.

(1) White: Carbon black / TiO ₂ /LDPE=0.2/2.5/97.3 (2) Chromatic color: Chromatic pigment / TiO ₂ / LDPE (or PP) = 0.5 / 5.0 / 94.5 (3) Black: Carbon black / TiO ₂ /LDPE=0.2/2.5/97.3 The compound of the above (1), (2) and (3) was kneaded with a heating two-roll roll for test for 5 minutes, and a press sheet having a thickness of 1 mm was prepared. To do. 0.5 mm of this 1 mm thick press sheet
The coloring strength is judged by simultaneous pressing of mm-thick press sheets. At this time, the display of the comparative product is set to 100.

Film Dispersion (Measurement of Number of Grids) An inflation film having a thickness of 30 μm is prepared, and the number of grids present in a film having a volume of 10 cc is measured. The compounding of the resin for measurement is as follows: colorant / high-pressure polyethylene, or colorant / polypropylene resin = 10/10
Compounded in a proportion of 0 Upper: grid size is 0.1 to 0.05 mm ² Lower: grid size is 0.05 to 0.01 mm ² Pressure increase ΔP Powder is the base material LDP
It shows the degree of kneading and dispersion in E or PP. As the kneading and dispersion is insufficient, the particulate pigment is more likely to be deposited on the screen, and as a result, the pigment is dispersed due to the change with time of the pressure generated on the upstream side of the screen. The degree of can be compared.

Explaining the test method, a single-screw extruder having a cylinder diameter of 15 mm and an L / D of 20 was sequentially loaded from the upstream side.
Five screens of 00, 250, 325, 250, and 100 mesh are arranged, 2.0 kg of master batch is melted, and pressure P ₁ (kg / cm ² ) and 2 after 3 minutes from starting to flow through the screen. The difference from the pressure P ₂ (kg / cm ² ) immediately before the end of the flow of the 0.0 kg masterbatch is determined. That is, the pressure increase ΔP (kg / c
m ² ).

ΔP = P ₂ −P ₁

[0050]

[Table 1] As is clear from Table 1, the specific examples 1 to 6 are
The coloring power, the film dispersion, and the pressure increase ΔP are excellent, whereas Comparative Examples 1 to 6 are poor in the coloring power, the film dispersion, and the pressure increase ΔP.

[0051]

Since the present invention is configured as described above, it has the following effects.

In the melting and kneading section, the resin material and the compounding agent are sheared and stretched by the interaction of a plurality of recesses formed on the inner wall surface of the cylinder and at least two kneading disks provided on the screw. It is melted and kneaded under the action, position exchange action and flow division action,
The compounding agent containing the colorant is finely and uniformly dispersed in the molten resin. As a result, it is possible to manufacture a colorant masterbatch that is continuous and has a high extrusion rate.

In addition, the pressure of the molten resin in the melting / kneading section is changed by adjusting the opening degree of the resin flow path in the cylinder by the flow path adjusting means, so that the kind of the resin material or the resin is kneaded. It has versatility to obtain melting and kneading characteristics corresponding to the type of compounding agent.

[Brief description of the drawings]

FIG. 1 is a schematic cross-sectional view showing an example of an apparatus for producing a colorant masterbatch of the present invention.

FIG. 2 is a schematic cross-sectional view taken along the line AA of FIG.

FIG. 3 is a schematic cross-sectional view taken along the line BB of FIG.

[Explanation of symbols]

 1 Colorant Masterbatch Manufacturing Device 2 Cylinder 3 Groove 4 Screw 5 Full Flight Part 6 Kneading Disc 7 Torpedo Ring 8 Slide Valve 9 Resin Flow Path 10 Supply Port 11 Vent Port 12 Cap

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Noriyoshi Oda 1-1-6 Funakoshi Minami, Aki-ku, Hiroshima City, Hiroshima Prefecture Japan Steel Works (72) Inventor Hideki Mizuguchi 1 Funakoshi-minami, Aki-ku, Hiroshima City, Hiroshima Prefecture 6th-1st Japan Steel Works, Ltd.

Claims (4)

[Claims] 1. A cylinder (2) and two meshing type screws (4) rotatably disposed in the cylinder (2), and at least a transport section (A, B) and a melting / melting section.
In a manufacturing apparatus for a colorant masterbatch including a kneading section (C) and an extruding section (E, F), a plurality of recesses are formed on the inner wall surface of the cylinder (2) at a portion corresponding to the melting / kneading section (C). The melting / kneading part (C) of the screw (4) is provided at a distance from each other.
At least two kneading discs (6) are provided at a portion corresponding to the resin passage (3) in the cylinder (2) between the melting / kneading section (C) and the extruding section (E, F). Flow path adjusting means (7, 8) for adjusting the opening degree of 9)
An apparatus for producing a colorant masterbatch, characterized in that 2. The plurality of recesses comprises a plurality of axially extending grooves (3) formed at intervals in the circumferential direction of the cylinder (2). Color masterbatch manufacturing equipment. 3. The apparatus for producing a colorant masterbatch according to claim 1, wherein the plurality of recesses are formed of a plurality of recesses formed at intervals from each other. 4. The flow path adjusting means comprises a torpedo ring (7) formed on the screw (4) and at least two slide valves (8) which can move forward and backward with respect to the torpedo ring (7). Moreover, the slide valves (8) are arranged at intervals in the circumferential direction of the cylinder (2).
An apparatus for manufacturing a colorant masterbatch according to the item.