JP2013000913A - Extruder and melting and kneading method using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide an extruder having high carrying efficiency of powdery filler and good dispersibility of the powdery filler and obtaining a resin composition with good physical properties.SOLUTION: A first kneading zone 3 located on the most upstream side of the extruder includes kneading blocks a-d in the following combination in this order from the upstream side: at least two sets of units each including at least one kneading block (a) and at least one kneading block b in this order; at least one kneading block (a) or at least one kneading block d; and at least one kneading block c, and a length of the kneading zone 3 is 6-15 times longer than a barrel diameter. In the kneading block (a), B/D=0.18-0.6, α=10-50°, and L/D=0.8-3.3, in the kneading block b, B/D=0.15-0.6, α=85-95°, and L/D=0.8-3.3, in the kneading block c, B/D=0.05-0.25, α=100-140°, and L/D=0.25-1.5, and in the kneading block d, B/D=0.05-0.17, α=10-50°, and L/D=0.45-0.75, wherein B, D, α and L indicate blade thickness, a screw diameter, a torsion angle between two blades adjacent to each other and length, respectively.

Description

  The present invention relates to an extruder, particularly an extruder suitable for melt-kneading a thermoplastic resin (particularly a pellet-like resin) and a powder filler, and melting of a thermoplastic resin and a powder filler using the extruder. The present invention relates to a kneading method.

Since the finer the powder filler contained in the resin composition, the better the balance between strength and toughness of the resin composition, the finer one is preferably used. However, on the other hand, if the powder filler is fine, the conveying efficiency of the powder filler in the extruder screw is lowered, and the dispersion of the powder filler in the resin composition is deteriorated, and the resin composition Physical properties are reduced.
Patent Document 1 discloses a technique for increasing the conveyance capability by combining powder resin or powder filler with only a single thread screw element, a clockwise kneading block, and a neutral kneading block.
Prior Document 2 discloses a technology for conveying powder resin by combining a powder filler and pellet resin with a single thread and a clockwise kneading block, and a neutral kneading block and a counterclockwise kneading block.

Japanese Patent Laid-Open No. 10-024483 JP-A-10-180842

  However, there is room for improvement in the screw configuration of the extruder that melts and kneads the above-described pellet-shaped resin and powder filler.

  As a result of intensive studies on an extruder used for melt-kneading a thermoplastic resin (particularly a pellet-shaped resin) and a powder filler, the present inventors have found that a special screw that arranges kneading blocks that satisfy specific conditions in a specific order. By adopting the configuration, it was found that even when the powder filler is fine, the conveyance efficiency by the extrusion screw is not lowered, and good dispersibility in the resin composition can be achieved, and the present invention has been completed.

That is, the present invention is as follows.
An extruder having at least one kneading zone,
In the first kneading zone located at the most upstream of the at least one kneading zone, the following kneading blocks (1) to (4) are arranged in order from the upstream, with at least one (1) and at least one ( Including at least two units comprising 2) in this order; including at least one unit of (1) or (4); comprising at least one unit of (3);
An extruder in which the length of the first kneading zone is 6 to 15 times its barrel diameter:
(1) Kneading block with B / D = 0.18-0.6, α = 10-50 degrees, L / D = 0.8-3.3,
(2) Kneading block with B / D = 0.15 to 0.6, α = 85 to 95 degrees, L / D = 0.8 to 3.3,
(3) Kneading block with B / D = 0.05 to 0.25, α = 100 to 140 degrees, L / D = 0.25 to 1.5,
(4) A kneading block having B / D = 0.05 to 0.17, α = 10 to 50 degrees, and L / D = 0.45 to 0.75.
(Where B and D are the thickness (mm) and screw diameter (mm) of the blades constituting the kneading block, α is the twist angle (degrees) between two adjacent blades, and L is the length of the kneading block Represents (mm).)

  According to the melt-kneading method of the present invention, even when a fine powder filler is melt-kneaded with a pellet resin, the powder filler can be transported with high transport efficiency, and the dispersibility of the powder filler is good, A resin composition having good physical properties can be obtained.

It is the schematic which shows the structure of the apparatus of this invention. It is the schematic which shows the outline | summary of the kneading block of this invention.

Hereinafter, the present invention will be described in detail.
FIG. 1 is a schematic view of an extruder according to the present invention.
The extruder of the present invention is preferably a twin-screw co-rotating extruder, and for example, ZSK series manufactured by COPPERION, TEM series manufactured by Toshiba Machine, Japan Steel Works TEX series, etc. are suitable.
The screw diameter of the kneading block included in the extruder is preferably in the range of 40 to 200 mm. By setting the screw diameter within the above range, it is possible to suppress excessive heat generation during melt-kneading while securing a high production amount and reducing costs.
The length of the extruder is preferably 12 to 60 times the screw diameter. By setting the length of the extruder within the above range, kneading can be sufficiently performed, and oxidation deterioration can be prevented.
Although there is no limitation in the motor used for an extruder, generally an inverter motor and a direct current motor are used. There are an air cooling type and a circulating water cooling type as the motor cooling method, but the circulating water cooling type is more preferable in order to prevent dust from being scattered in the air.

In the extruder of the present invention, the raw materials (for example, pellet-shaped resin and powder filler) supplied from a first supply port provided upstream from the first kneading zone pass through the solid conveying zone to the first kneading zone. It is conveyed to. In this transport zone, generally one or two screws are used as screw elements. The length of the screw element used in the conveyance zone is generally about 0.3 to 3.3 times the screw diameter. When a single thread is used, the conveying ability is higher than that of a double thread, but the double thread is preferable in view of the wear of the screw element.
The most upstream position of the first kneading zone is preferably in the range of 5.0 to 32 times the screw diameter from the center of the barrel (No. 1 barrel) provided with the first supply port.

In the extruder of the present invention, in the first kneading zone located at the most upstream (when there is one kneading zone, the only kneading zone is the first kneading zone), the screw has a plurality of types of knees. And has a characteristic in its configuration (combination and order). The kneading block is also referred to as a kneading disk, and refers to a screw element having a configuration in which a plurality of blades having substantially the same shape are sequentially shifted at a substantially constant angle around the central axis of the screw. FIG. 2 shows a schematic diagram of a specific example (having five blades).
That is, the extruder according to the present invention includes the following kneading blocks (1) to (4) in the first kneading zone located at the most upstream among the at least one kneading zones in order from the upstream. (1) and at least one unit comprising at least one (2) in this order; at least two units; comprising (1) or (4) at least one; (3) comprising at least one order;
The length of the first kneading zone is 6 to 15 times the barrel diameter.
(1) Kneading block with B / D = 0.18-0.6, α = 10-50 degrees, L / D = 0.8-3.3,
(2) Kneading block with B / D = 0.15 to 0.6, α = 85 to 95 degrees, L / D = 0.8 to 3.3,
(3) Kneading block with B / D = 0.05 to 0.25, α = 100 to 140 degrees, L / D = 0.25 to 1.5,
(4) Kneading block with B / D = 0.05 to 0.17, α = 10 to 50 degrees, and L / D = 0.45 to 0.75

As an example of the arrangement of the kneading blocks (1) to (4),
(1), (2), (1), (2), (1), (3);
(1), (2), (1), (2), (4), (3);
(1), (1), (2), (2), (1), (1), (2), (2), (1), (3);
(1), (1), (2), (2), (1), (1), (2), (2), (4), (3);
(1), (1), (2), (2), (1), (1), (2), (2), (1), (4), (3), (3);
(1), (1), (1), (2), (2), (2), (1), (1), (1), (2), (2), (2), (1 ), (1), (3) and the like.
Where B and D are the thickness (mm) and screw diameter (mm) of the blades constituting the kneading block, α is the twist angle (degrees) between two adjacent blades, and L is the length of the kneading block (Mm).

Here, the thickness B of the blade is a value (average value) obtained by dividing the length L of the kneading block by the number of blades constituting the kneading block, and the screw diameter D is the shape of the blade being an ellipse. In some cases, the major axis is longer, and in the case where the shape of the blade is not an ellipse, it is the long side of the circumscribed rectangle that minimizes the area circumscribing the blade (see FIG. 2).
The number of blades constituting each kneading block is 2 or more, preferably 2 to 10, more preferably 3 to 8, and further preferably 3 to 7.
The twist angle α is an angle formed by adjacent blades (see FIG. 2).

  In the first kneading zone, four types of kneading blocks satisfying the above conditions for B / D, α, and L / D are used in combination in a specific order, and the length of the first kneading zone is set to the barrel diameter. By making it 6 to 15 times as large as this, the ability to convey the powder filler (especially fine powder filler) of the extruder is improved, and the dispersibility of the powder filler in the produced resin composition is improved. .

  The length L of the kneading block and the ratio L / D of the screw diameter D and the length L of the kneading block can be freely changed by changing the number of blades constituting the kneading block.

The screw configuration in the first kneading zone of the present invention includes at least the kneading blocks (1) to (4) as described above, but may appropriately include other kneading blocks. .
For example, a kneading block of α = 10 to 50 degrees and B / D = 0.05 to 0.25 may be arranged on the most downstream side of the first kneading zone so as not to reduce the conveying capacity.

  An atmospheric vent and / or a vacuum vent may be arranged downstream of the first kneading zone. These vents are effective for removing gas contained in the powder filler, volatile matter of the thermoplastic resin, decomposition products, and the like. From such a viewpoint, the absolute pressure of the vacuum vent is preferably 0.05 to 0.9 MPa. When installing a vacuum vent, use a kneading block or reverse screw similar to the kneading block in (3) to melt-seal the downstream side of the vacuum vent with resin (in order to fill 100% with molten resin). Is preferred.

  When there are a plurality of kneading zones, a second supply port and a third supply port for supplying the thermoplastic resin and filler from the side can be provided downstream of the first kneading zone. In this case, the second and third supply ports are preferably provided in a barrel (side feed barrel) connected downstream of the barrel constituting the first kneading zone, and side feeders are installed in the second and third supply ports. It is preferred that The side feed barrel is preferably provided with a venting vent. A second kneading zone is provided downstream of the second and third supply ports. There is no limitation on the kneading means used in the second (third) kneading zone. For example, the above kneading blocks (1) to (3), reverse screws and the like are arbitrarily used.

  A die plate can be installed at the tip of the die part of the extruder. The hole diameter of the strand of the die plate can be, for example, about 1.5 to 6.0 mm, and the number of holes can be adjusted so that the flow rate is about 10 to 40 kg / hr per hole. In the case of the strand cut method, a scum may be generated at the strand outlet of the die plate. Therefore, a scouring device for blowing air may be installed. At that time, the air used should be passed through a filter having a pore diameter of about 5 μm. The cooling water of the strand bath should be passed through a filter having a pore diameter of about 10 μm. Moreover, it can replace with a strand cut system and a hot cut system and an underwater cut system can also be employ | adopted. The pellet obtained by the strand cut method is cylindrical. On the other hand, the pellets obtained by the hot cut method and the underwater cut method are spherical or elliptical. The target average size of the pellets can be set to 1-6 mm. More preferably, it is 2-5 mm, More preferably, it is 2.5-3.5 mm. Pellets whose cutting target value is set to 1 to 6 mm can be sufficiently kneaded with a molding machine screw or an extruder screw.

Hereinafter, materials suitable for kneading using the extruder of the present invention will be described.
The extruder of the present invention is suitable for melt-kneading a thermoplastic resin and a filler.
Examples of the thermoplastic resin suitable for kneading using the extruder of the present invention include, for example, polyphenylene ether, a blend of polyphenylene ether and polystyrene resin, polystyrene resin (general purpose polystyrene, high impact polystyrene, acrylonitrile and styrene). Copolymer), polycarbonate, polyolefin resin, homopolyoxymethylene, copolymer polyoxymethylene, polyphenylene sulfide, polyamide resin, polyamideimide, polyarylate, polyarylsulfone, polyethersulfone, polyetherimide, poly Examples thereof include at least one resin selected from tetrafluoroethylene and polyether ketone. A preferred thermoplastic resin is at least one selected from a blend of polyphenylene ether and alkenyl resin, polystyrene resin, polycarbonate, polyolefin resin, polyphenylene sultide and polyamide resin. Further preferred thermoplastic resins are a blend of polyphenylene ether and polystyrene resin and polystyrene resin. The blend may be a dry blend of polyphenylene ether and polystyrene resin, or a concentrate obtained by melt-kneading polyphenylene ether and polystyrene resin.

  The extruder of the present invention is particularly suitable for kneading a pellet-shaped resin obtained by molding the above thermoplastic resin into pellets such as a cylinder, a sphere, and an ellipsoid. In the case of a cylindrical pellet, the size of the pellet is preferably 1 to 6 mm in diameter and 1 to 6 mm in length, and is usually about 3 mm in diameter and about 3 mm in length. The size of the spherical pellet is preferably 1 to 6 mm in diameter, usually about 3 mm in diameter, and the oval pellet is elliptical with an aspect ratio of 0.5 to 0.9, and 1 to 6 mm in length and width. It is preferable that it is 2-4 mm normally.

Examples of the filler suitable for kneading with the above-described thermoplastic resin using the extruder of the present invention include, for example, glass fiber, carbon fiber, metal fiber, potassium titanate whisker, magnesium sulfate whisker, aluminum borate whisker, and carbonic acid. Calcium whisker, silicon carbide whisker, zinc oxide whisker, calcium silicate (wollastonite), mica, talc, glass flake, calcium carbonate, clay, kaolin, barium sulfate, silica, alumina, magnesium oxide, magnesium sulfate There is at least one kind.
Among these, in particular, potassium titanate whisker, magnesium sulfate whisker, aluminum borate whisker, calcium carbonate whisker, silicon carbide whisker, zinc oxide whisker, calcium silicate (warastite), mica, talc, At least one powder filler selected from glass flakes, calcium carbonate, clay, kaolin, barium sulfate, silica, alumina, magnesium oxide, and magnesium sulfate is preferred.
More preferable powder fillers are talc and calcium carbonate, and more preferable powder fillers are talc and calcium carbonate having an average particle size of 5 μm or less. The average particle size of the powder filler is obtained by measuring the maximum length of a projected image of 100 arbitrary powders on an image such as an optical microscope or a scanning electron microscope, and obtaining the average value. It is.

  When kneading a thermoplastic resin and a filler using the extruder of the present invention, the kneading ratio of the thermoplastic resin and the filler is 40 to 90 wt% of the thermoplastic resin with respect to a total of 100 wt% of the thermoplastic resin and the filler. %, The filler is preferably 60 to 10% by weight, more preferably 50 to 85% by weight of the thermoplastic resin, 50 to 10% by weight of the filler, and still more preferably 60 to 10% by weight of the thermoplastic resin. %, Filler 40 to 10% by weight.

When the thermoplastic resin composition is produced using the extruder of the present invention, at least 20% by weight (preferably 30% by weight or more, more preferably 40% by weight or more) of 40 to 90% by weight of the thermoplastic resin. Is preferably subjected to melt kneading in a pellet form (as a pellet-like resin).
Further, it is preferable that at least 1% by weight (preferably 5% by weight, more preferably 10% by weight) of 50 to 10% by weight of filler is provided as powder.

  When melt-kneading using the extruder of the present invention, in addition to the thermoplastic resin and filler, a powder filler dispersant (ethylene bisamide, calcium stearate, zinc stearate, stearic acid), elastomer, oil (Paraffinic, naphthenic, silicon-based), functional group imparting agent (maleic acid, fumaric acid, itaconic acid, maleic anhydride, malic acid, citric acid), various colorants, coloring additives (such as titanium oxide), ultraviolet rays Absorbers, antistatic agents, stabilizers (zinc oxide, zinc sulfide, phosphorous, sulfur, hindered phenol, etc.) can be added.

Hereinafter, the present invention will be further described with reference to examples and comparative examples.
In Examples and Comparative Examples, TEM58SS (12 barrels) (biaxial co-rotating extruder) manufactured by Toshiba Machine Co., Ltd. was used as an extruder. (See Figure 1)
The barrel configuration is as follows.
No. 1 barrel: A first supply port is provided.
No. 2 barrels: transfer zone no. 3 to 4 barrels: First kneading zone No. 5 barrels: An air vent is provided.
No. 6 barrels: A second supply port is provided. (Side feed barrel)
No. 7 barrel: Second kneading zone No. 8 barrels: A third supply port is provided. (Side feed barrel)
No. 9 barrels: No. 3 kneading zone 10 barrels: A vacuum vent (absolute pressure 0.01 MPa) is provided.
No. 11, 12 barrels: closed barrel Other conditions are as follows.
Die plate: 4Φmm Orifice length 15mm 20 holes Strand bath: Water temperature 40 ℃ ± 3 ℃
Pelletizer: Columnar diameter target value 2.5 ± 0.3mm
Vibrating sieve: Installed on the downstream side of the pelletizer to eliminate long pellets, continuous pellets and chips All barrel temperatures), die temperature: 280 ° C

  A weight type feeder A for pelletized resin and a weight type feeder B for powder filler were installed in the first supply port. A side feeder was attached to the second supply port, and a weight type feeder C for pellet resin and a weight type feeder D for powder filler were arranged. The side feeder was attached to the 3rd supply port, and the weight type feeder E for glass fibers was arrange | positioned.

(Filler dispersibility evaluation)
The appearance of the surface of the pin gate portion of a flat plate obtained by injection molding a flat plate having a length of 200 mm × width 200 mm × thickness 2 mm was measured by an injection molding machine.
The filler dispersibility was evaluated in five stages of 1 to 5 based on the following criteria.
1: 75% or more of the surface radius within 1 cm from the center of the pin gate portion is rough.
2: Similarly, 50 to 74% within a radius of 1 cm is rough.
3: Similarly, 25 to 49% within a radius of 1 cm is rough.
4: Similarly, 1 to 24% within a radius of 1 cm is rough.
5: Similarly, there is no roughness within a radius of 1 cm.

(Powder filler penetration)
It was visually observed whether the powder filler was deposited on the extruder screw at the bottom of the first supply port.

(Evaluation of the physical properties)
Using the pellets produced by the extruder, a flat plate having a length of 200 mm × width of 200 mm × thickness of 2 mm was formed with an injection molding machine (IS-80AM injection molding machine manufactured by Toshiba Machine). The cylinder temperature at that time was 240 to 290 ° C., and the mold temperature was 60 to 90 ° C. About the obtained molded object, Izod impact strength and tensile elongation were measured. Izod impact strength was evaluated according to ASTM D256 as a 1/8 inch notched short rail. Tensile elongation was evaluated with a 1/8 inch dumbbell according to ASTM D658.

(Kneading block)
In the examples and comparative examples, eight types of kneading blocks A to H shown in Table 1 were used.
Among them, A and B are the kneading block (1) of the present invention, D and E are the kneading block (2) of the present invention, G and H are the kneading block (3) of the present invention, and C is the present invention. (4)

[Examples 1 to 4, Comparative Examples 1 to 8]
With the screw configuration of the extruder shown in Table 2, melt kneading was performed to produce a resin composition.
In Examples 1 to 4 and Comparative Examples 1 to 8, only the screw configuration was changed as shown in Table 2, and all other conditions were the same.
The kneaded raw material was 31.5 parts by weight of polyphenylene ether S201A (manufactured by Asahi Kasei Plastics Singapore) (hereinafter PPE) / general purpose polystyrene 685 (manufactured by PS Japan) (hereinafter 685) = 80/20 concentrate pellets, 685 23 parts by weight, 25 parts by weight of high impact polystyrene H9302 (manufactured by PS Japan), 0.5 parts by weight of Toughmer P0680J (manufactured by Mitsui Kagaku), 0.2 parts by weight of ethylene bissterial amide (manufactured by Kao), average particle 20 parts by weight of 4 μm diameter talc (Hytron A) (manufactured by Takehara Kogyo).
All raw materials other than talc were blended with a tumbler, then transferred to a moving hopper, and supplied from the weight feeder A to the first supply port at 320 kg / hr.
Talc was put into the weight type feeder B and supplied to the first supply port at 80 kg / hr. The results of Examples 1 to 4 and Comparative Examples 1 to 8 are shown in Table 3.

  In Examples 1 to 4, talc penetration was good, talc dispersibility in the resin composition was good, and physical properties of the resin composition were also good.

Since Comparative Example 1 (screw configuration 2) includes (1) and (3), the bite property of talc is good and the resin composition temperature near the die outlet is low, but does not include (2). Compared to the Examples, the dispersibility of talc was poor, and the physical properties of the resin composition were not good.
In Comparative Example 2 (screw configuration 3), the repeated unit is not a combination of (1) and (2), but a combination of (1) and (3). The amount of extrusion decreased. Furthermore, the resin composition temperature in the vicinity of the die exit was high, and the physical properties of the resin composition were not good.
In Comparative Example 3 (screw configuration 4), since the unit containing (1) and (2) is repeated once, the talc dispersibility is poor compared to the examples, and the physical properties of the resin composition are also not good. There wasn't.

In Comparative Example 4 (screw configuration 5), the order of the combination of the units including (1) and (2) does not satisfy the conditions of the present invention. However, the dispersibility of talc was low, and the physical properties of the resin composition were not good accordingly.
In Comparative Example 5 (screw configuration 6), since the unit including (1) and (2) is repeated only once (because the following (1) and (2) are reversed), compared to the example, Talc bite was poor, the amount of extrusion was low, talc dispersibility was poor, and the physical properties of the resin composition were not good.

In Comparative Example 6 (screw configuration 7), the combination of (1) to (3) is satisfied, but the length of the first kneading zone is short (less than 6 times the barrel diameter), so compared to the examples, The talc dispersibility was poor, and the physical properties of the resin composition were not good.
Comparative Examples 7 and 8 (screw configurations 8 and 9) do not have a unit including (1) and (2) (repeated units do not correspond to (4) and F ((2))) Because of the combination), the talc dispersibility is lowered and the physical properties are also lowered as compared to the examples.
From the comparison between Examples and Comparative Examples, if the screw configuration of claim 1 is used, a resin composition having satisfactory physical properties can be obtained while satisfying productivity and dispersibility of the powder filler.

[Examples 5 and 6]
Melt-kneading was carried out under the same conditions as in Example 1 except that the talc dispersant in Example 1 was replaced with zinc stearate and calcium stearate. As in Example 1, the penetration of talc was good, the dispersibility of talc was good, and the physical properties of the resin composition were also good.
[Example 7]
Melt-kneading was performed under the same conditions as in Example 1, except that 10 parts by weight (40 kg / hr each) of talc was supplied to the weight feeder B at the first supply port and the weight feeder D at the second supply port. As in Example 1, the penetration characteristics of talc were good, and the physical properties of the resin composition were also good except that the dispersibility of talc was slightly lower (5 to 4).
[Example 8]
H9302 The supply position of 25 parts by weight is changed and supplied from the weight type feeder C to the second supply port, and the supply position of 10 parts of talc is changed and supplied from the weight type feeder E to the third supply port. Melt kneading was performed under the same conditions as in Example 7. As a result of the side feed of H9302, heat deterioration of the rubber component could be prevented, and as a result, the Izod impact strength of the resin composition was good.
[Example 9]
Melt kneading was carried out in the same manner as in Example 1 except that the powder filler was changed to calcium carbonate (Softon 2200, average particle size 1 μm, manufactured by Shiraishi Calcium Co., Ltd.). As in Example 1, the bite property of calcium carbonate was good, and the physical properties of the resin composition were also good except that the dispersibility of talc was slightly lower (5 to 4).
[Example 10]
Melt kneading was carried out in the same manner as in Example 1 except that the powder filler was changed to talc (RGE 250 average particle size 2 μm, manufactured by Fuji Talc Kogyo Co., Ltd.). As in Example 1, the penetration characteristics of talc were good, and the physical properties of the resin composition were also good except that the dispersibility of talc was slightly lower (5 to 4).
[Example 11]
Melt kneading was carried out under the same conditions as in Example 7 except that a glass fiber chop (manufactured by Nippon Sheet Glass Co., Ltd.) having a thickness of 13 μm and a length of 3 mm was used instead of talc supplied to the second supply port. The physical properties of the obtained resin composition were also good.

[Comparative Example 9]
Melt kneading was performed under the same conditions as in Example 11 except that the screw configuration of the first kneading zone was changed to 2. Compared with Example 11, the physical property of the resin composition fell.
[Example 12]
Melt-kneading was carried out under the same conditions as in Example 8 except that a glass fiber chop (manufactured by Nippon Sheet Glass Co., Ltd.) having a thickness of 13 μm and a length of 3 mm was used instead of talc supplied to the third supply port. The physical properties of the resin composition were also good.
[Comparative Example 10]
Melt kneading was performed under the same conditions as in Example 11 except that the screw configuration of the first kneading zone was changed to 2. Compared with Example 12, the physical property of the resin composition fell.

[Example 13]
Melt-kneading was carried out under the same conditions as in Example 1 except that polycarbonate L1250Y (manufactured by Teijin Kasei Co., Ltd.) was used as the pellet-shaped resin instead of PPE / 685 concentrate. As in Example 1, the penetration of talc was good, the dispersibility of talc was good, and the physical properties of the resin composition were also good.
[Example 14]
Melt-kneading was performed under the same conditions as in Example 1 except that 1300S of nylon 6,6 (manufactured by Asahi Kasei Chemicals) was used as the pellet-shaped resin instead of PPE / 685 concentrate. As in Example 1, the penetration of talc was good, the dispersibility of talc was good, and the physical properties of the resin composition were also good.

  As confirmed in the above examples, when the extruder of the present invention is used, a satisfactory dispersibility of the powder filler can be achieved while maintaining the powder filler conveying ability, and a resin composition having good physical properties can be obtained. I can do it.

  Since the resin composition obtained by the extruder or the melt-kneading method of the present invention has good dispersibility of the powder filler and good physical properties, OA materials (printers, copying machines, etc.), electronic materials, optical materials, It can be suitably used for battery case materials, battery cell materials, films, sheets and the like.

(1) Extruder body (2) First supply port (3) First kneading zone (4) Vacuum vent or atmospheric vent (5) Second supply port (6) Second kneading zone (7) Third supply port ( 8) Third kneading zone (9) Vacuum vent or atmospheric vent

Claims (9)

An extruder having at least one kneading zone,
In the first kneading zone located at the most upstream of the at least one kneading zone, the following kneading blocks (1) to (4) are arranged in order from the upstream, with at least one (1) and at least one ( Including at least two units comprising 2) in this order; including at least one unit of (1) or (4); comprising at least one unit of (3);
An extruder in which the length of the first kneading zone is 6 to 15 times its barrel diameter:
(1) Kneading block with B / D = 0.18-0.6, α = 10-50 degrees, L / D = 0.8-3.3,
(2) Kneading block with B / D = 0.15 to 0.6, α = 85 to 95 degrees, L / D = 0.8 to 3.3,
(3) Kneading block with B / D = 0.05 to 0.25, α = 100 to 140 degrees, L / D = 0.25 to 1.5,
(4) A kneading block having B / D = 0.05 to 0.17, α = 10 to 50 degrees, and L / D = 0.45 to 0.75.
(Where B and D are the thickness (mm) and screw diameter (mm) of the blades constituting the kneading block, α is the twist angle (degrees) between two adjacent blades, and L is the length of the kneading block Represents (mm).)   The extruder according to claim 1, comprising at least one atmospheric vent and / or vacuum vent downstream from the first kneading zone.   Furthermore, the extruder of Claim 1 or 2 which has a 2nd supply port and a 2nd kneading | mixing zone in this order downstream from said 1st kneading | mixing zone.   Furthermore, the extruder of Claim 3 which has a 3rd supply port and a 3rd kneading | mixing zone in this order downstream from said 2nd kneading | mixing zone.   The melt-kneading method including the process of melt-kneading at least a thermoplastic resin and a filler using the extruder of any one of Claims 1-4.   The kneading ratio of the thermoplastic resin and the filler is 40 to 90% by weight of the thermoplastic resin and 60 to 10% by weight of the filler with respect to a total of 100% by weight of the thermoplastic resin and the filler. The melt kneading method according to claim 5.   The thermoplastic resin is a polystyrene resin, polyphenylene ether, polycarbonate, polyolefin resin, homopolyoxymethylene, copolymer polyoxymethylene, polyphenylenesulfide, polyamide resin, polyamideimide, polyarylate, polyarylsulfone, polyether The melt-kneading method according to claim 5 or 6, wherein the melt-kneading method is at least one selected from the group consisting of sulfone, polyetherimide, polytetrafluoroethylene, and polyetherketone.   The filler is glass fiber, carbon fiber, metal fiber, potassium titanate whisker, magnesium sulfate whisker, aluminum borate whisker, calcium carbonate whisker, silicon carbide whisker, zinc oxide whisker, calcium silicate (wollastonite), mica, The melting according to any one of claims 5 to 7, which is at least one selected from talc, glass flake, calcium carbonate, clay, kaolin, barium sulfate, silica, alumina, magnesium oxide, and magnesium sulfate. Kneading method.   The thermoplastic resin is a pellet-shaped resin composed of 10 to 90 parts by weight of a blend of polyphenylene ether and polystyrene resin and 90 to 10 parts by weight of a polystyrene resin, and the filler is talc having an average particle size of 5 μm or less. The melt-kneading method as described in any one of Claims 5-8 which exists.