JPH1024483A - Extruder for powder and extrusion method using the same - Google Patents

Abstract

(57) [Abstract] [Purpose] For a powder extruder, stabilize torque and improve extrusion efficiency without causing unmelted resin to mix or vent up. [Structure] The screw structure of the solid transport zone is as follows: (A) having an overall length of L / D = 4.5 to 23;
/D=1.5 to 9 (B) below, the total combination length is L / D = 9 to 32, and the screw configuration of the first kneading zone is the following (C) and (D). Combination. (A): A screw element having a screw flight angle of 100 to 200 degrees and a length L / D = 0.9 to 2.0. (B): A screw element having a screw flight angle of 10 to 25 degrees and a length L / D = 0.9 to 2.0. (C) The twist angle is 80-100 degrees and the length is L /
K = kneading disk of 0.2-2.0. (D) The twist angle is 15 to 65 degrees and the length is L / D
= Kneading disc of 0.4-2.0.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an extruder suitable for melting and kneading a powdery resin alone or a powdery resin and a powdery reinforcing material and / or a pellet-like resin and extruding the same. The present invention relates to a method for melting, kneading and extruding a powdery resin alone or a powdery resin and a powdery reinforcing material and / or a pellet-like resin using an extruder.

[0002]

2. Description of the Related Art In general, a powdery resin is used alone or in combination with a powdery reinforcing material and / or a pellet-like resin.
After being granulated through an extruder, it is used for production of products by a molding machine.

[0003] By the way, powdery resin has a property that biting into a screw of an extruder is worse than that of pellet-shaped resin. The smaller the apparent specific gravity and the smaller the average particle diameter of the powdery resin, the worse the extruder bites into the screw, and the productivity of the granulated product decreases. Similarly, the productivity of the granulated material also decreases when the powdery reinforcing material and / or the pellet-like resin are simultaneously supplied with the powdery resin. The extrusion technique of such a powdery resin alone or a mixture of the powdery resin and a powdery reinforcing material and / or a pellet-like resin is an important technique in molding, but few techniques have been published so far.

Conventionally, the following are known as powder extrusion techniques.

(1) According to the technical data of the German company Warner & Friedler, when extruding the powdery resin, the screw configuration of the first kneading zone of the extruder falls within the category of (D) in the present invention. It is disclosed that there is only a kneading disc to be inserted.

(2) Japanese Patent Application Laid-Open No. 02-1650 discloses that at least one vent port is provided, and that kneading and extrusion are performed without compression in the first kneading zone.

(3) The following technology is disclosed in the "Journal of the Japan Society of Molding and Processing 96th Annual Conference B211" published on June 7, 1996 regarding extrusion experiments of polypropylene and talc. That is, in the solid transport zone, a screw element that falls within the category of (A) of the present invention has a length of about L / D.
= 5 and a screw element having a length of about L / D = 1 in the category of (B) of the present invention, while the first kneading zone falls in the category of (D) of the present invention. With respect to an extruder provided with a needing disk and arranged with a neutral falling in the category of (C) of the present invention at the most downstream of the first kneading zone, the extrusion amount and the rotation speed of polypropylene and talc, or the particle size and amount of talc The ratio is being considered. However, changes in the amount of extrusion when the screw configuration was changed were not examined. Regarding the vent position and number, the vent immediately after the first kneading zone is open to the atmosphere, and the vent immediately after the second kneading zone is a vacuum vent.

[0008]

However, in the case of the screw constitutions (1) and (2), the resin pressure does not increase in the first kneading zone, so that the extrusion rate is improved, but the kneading power is insufficient and the powder is insufficient. It is difficult to completely melt the body resin, and the unmelted resin is mixed and extruded, the dispersion of the powdery reinforcing material is reduced, and vent-up is likely to occur.
That is, kneading may be insufficient. Further, if the properties of the powder change or the amount of the powder and the pellets in the pellet system increases, there is a problem that insufficient kneading is caused and vent-up is easily caused. Further, since the powder is fluidized in the transport zone, there is a problem that the powder transport becomes unstable and the fluctuation of the torque increases.

In the report based on the screw configuration of (3), extrusion in a polypropylene / talc system is described.
Although the amount of extrusion is described, the state of dispersion of talc is not described. Further, according to the knowledge of the present inventor, in the above (3), in the method of assembling the screw elements (A) and (B), the optimum productivity may not always be obtained as the powder transport zone screw configuration.
In addition, in the extrusion of powder and pellet-like resin, if the amount of pellets increases, the screw configuration of the kneading zone in (3) may cause insufficient kneading, venting up, or poor dispersion. is there. Moisture and volatile matter contained in the pellets of the powdered resin material and powder reinforcing material may cause molding defects such as silver when the extruded pellets are injection-molded. There is. In other words, prevent vent up with a vacuum vent,
In addition, sufficient kneading is necessary to remove volatile components and moisture.

According to the present invention, especially in the powder extruding process, it is possible to stabilize torque fluctuation without causing trouble due to insufficient kneading such as mixing of unmelted resin, venting up, and removal of volatile components, and extruding efficiency. It is an object of the present invention to improve the productivity of pelletized resin and the like performed through the extrusion.

[0011]

According to the present invention, there is provided:
In the twin-screw extruder, the screw configuration of the solid transport zone is a combination of the following screw element (A) having an overall length of L / D = 4.5 to 23 and an overall length of L / D =
1.5 to 9 of the following screw element (B) combinations, and the total combination length of (A) and (B) is L / D = 9 to 32. The powder extruder is characterized in that the screw is constituted by a combination of a screw part (C) and a kneading disk (D) described below.

(A): Screw flight angle is 100
~ 120 degrees and the screw lead length is L / D = 0.
9 to 2.0 screw elements.

(B): Screw flight angle is 10
25 degrees and screw lead length L / D = 0.9 ~
2.0 screw element.

(C): a kinding disk selected from a needing disk having a twisting angle of 80 to 100 degrees, a needing disk having a twisting angle of -10 to 10 degrees, and a mixing screw in which a mountain portion of the screw is notched. Screw parts and the screw part length is L / D =
0.2-2.0 screw parts.

(D): when the twist angle is 15 to 65 degrees,
And the length of the needing disk is L / D = 0.4 ~
2.0 needing disc.

Further, the present invention is suitable for extruding a powdery resin alone or a mixture of a powdery resin with a powdery reinforcing material and / or a pellet-like resin using this powder extruder. And an extrusion method.

[0017]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described with reference to FIGS.

The present powder extruder 1 is a twin-screw extruder that can obtain a sufficient conveying force for powdery resin and powdery reinforcing material. Good, but generally co-rotating.

The present powder extruder 1 is generally used for obtaining a pellet-shaped resin, but the present invention is not limited to this, and even if a sheet or film can be formed. Good. For example, ZSK series manufactured by Warner & Friedler, TEM manufactured by Toshiba Machine Co., Ltd.
The extruder for powder of the present invention can be obtained by improving the screw configuration in the first kneading zone such as a series or a TEX series manufactured by Nippon Steel Corporation.

The length of the powder extruder 1 is L / D
(L = length, D = screw diameter) is preferably 10 to 60. When the L / D is less than 10, degassing and side feed are difficult to perform, and when the L / D exceeds 60,
The residence time of the resin is prolonged, and the resin is likely to deteriorate.

In the present invention, the screw structure of the solid conveying zone and the screw structure of the first kneading zone are particularly characterized. This solid transport zone is shown in FIG.
The powdery resin supplied from the main hopper 2 or a mixture of the powdery resin and the powdery reinforcing material and / or pelletized resin is conveyed to the first kneading zone. The first kneading zone is a region where the conveyed powdery resin or a mixture of the powdery resin and the powdery reinforcing material and / or pelletized resin is first kneaded, and is the length of the extruder 1 for powder. Although it depends, the L / D of the present powder extruder is in the range of 9.0 to 32.0 from the center position of the barrel where the main hopper 2 is provided.

The screw configuration of the solid transport kneading zone in the present invention comprises a combination of a screw element (A) described later and a combination of a screw element (B).

The screw element (A) used in the present invention
As shown in FIG. 2, is generally called a single thread. The screw lead length L / D of the screw element (A) needs to be 0.9 to 2.0. If the L / D is less than 0.9, the carrying capacity is reduced,
If the L / D exceeds 2.0, the carrying capacity is too large, causing troubles such as surging.

The screw flight angle α of the screw element (A) needs to be 100 to 120 degrees. When the screw flight angle α exceeds 120 degrees, the space area of the screw decreases, and the carrying capacity decreases. If the screw flight angle α is less than 100 degrees, the screw space area will increase and the transfer capacity will increase, but the space area will be too large, and the wall thickness of the screw shaft and the screw valley will be too thin. The target strength decreases.

The length for assembling the screw element (A) is
It is necessary that L / D = 4.5-23. L / D
Is less than 4.5, it is not possible to obtain the stability of the transfer capacity and the torque. Further, even if the L / D exceeds 23, no further improvement in the transport capacity can be expected.

Screw element (B) used in the present invention
As shown in FIG. 3, is generally called a double thread screw. The screw lead length L / D of the screw element (B) needs to be 0.9 to 2.0. If the L / D is less than 0.9, the carrying capacity is reduced,
If the L / D exceeds 2.0, the carrying capacity is too large, causing troubles such as surging.

The screw flight angle α of the screw element (B) needs to be 10 to 25 degrees. If the screw flight angle α exceeds 25 degrees, the space area of the screw decreases, and the carrying capacity decreases. If the screw flight angle α is less than 10 degrees, the screw space area will increase and the transfer capacity will increase, but the space area will be too large, and the wall thickness of the screw shaft and screw valley will be too thin. The target strength decreases.

The length for assembling the screw element (B) is
L / D = 1.5-9 is preferable, and when L / D is less than 1.5, the improvement of the carrying capacity cannot be obtained. Also, L / D is 9
No further improvement in transport capacity can be expected.

Screw element (A) used in the present invention
And the total combination length L / D of (B) needs to be 9.0 to 32. If the L / D is less than 9.0, an improvement in the transport capacity cannot be obtained depending on the resin. Also, L /
Even if D exceeds 32, no further improvement in transport capacity can be expected. A space ring or a screw element connecting (A) and (B) is installed between the screw elements (A) and (B), but the total combination length of the screw elements (A) and (B) is The length of the space ring and the connecting screw element shall not be included.

The screw structure of the solid transport zone in the present invention is a combination of at least one of the above screw elements (A) and at least one of the above screw elements (B). By this combination, an improvement in the transfer capacity and a stabilization of the torque fluctuation can be obtained, and the extrusion efficiency can be improved.

The first kneading zone of the present powder extruder 1 is
It is composed of a combination of one or more kinds of screw parts (C) and one or more kinds of kneading discs (D).

As the screw part (C) used in the present invention, a kneading disk as shown in FIG. 5 in which the twist angle θ of the blade 3 is 80 to 100 degrees,
Preferably, the number of the blades 3 is two or more, and the twist angle θ is 90.
Degree (neutral), the twist angle θ of the blade 3 is −
10 to 10 degrees, preferably one blade 3 and a twist angle θ of 0 degrees or 180 degrees (wide), and further cut out a screw mountain (flight portion) as shown in FIG. Mixing screw (notched mixing screw with a forward feed two-thread screw, or reverse-feed single-thread notch mixing screw, etc.). It is preferable that the number of the notches 11 is 8 to 20 per screw lead. The mixing screw also includes a gear-type mixing screw.

The length L / D of the screw part (C) is equal to 0.
It needs to be 2 to 2.0. When L / D exceeds 2.0, a strong shearing force is generated, causing deterioration of the resin and destruction of the screw parts. When L / D is less than 0.2, the mechanical strength of the screw becomes weak.

The kneading disk (D) used in the present invention has a twisting angle θ of the blade 3 of the kneading disk shown in FIG. 5 of 15 to 65 degrees (kneading light). Generally, the twist angle θ of the blade 3
Is preferably 30 degrees, 45 degrees or 60 degrees, and the number of blades 3 is preferably two or more. The length L / D of the needing disk (D) needs to be 0.9 to 2.0. When L / D exceeds 2.0, a strong shearing force is generated, which causes deterioration of the resin and breakage of the screw parts,
When L / D is less than 0.4, the mechanical strength of the screw becomes weak. .

In the present invention, the first kneading zone preferably has a screw configuration (E). In this screw configuration (E), in the first kneading zone, the thickness of one blade is L / D =
This is a screw configuration in which one or more 0.07 to 0.2 needing disks are arranged at the most downstream of the first kneading zone.

The thickness T per one blade is simply expressed by equation (1).

[0037]

[Equation 1] Blade thickness T = (length of nipping disk)
/ (Number of blades x screw outer diameter)

The thickness T of one blade is L / D = 0.07.
The needing disk of ~ 0.2 is set at the most downstream of the kneading zone. The effect is that by increasing the filling rate at the most downstream of the first kneading zone, a short path of the resin from the first kneading zone is prevented, so that sufficient kneading performance can be obtained even if the maximum pressure during filling is low. Can be for that reason,
In the case of a dinging disc having a blade thickness exceeding L / D = 0.2, the filling rate does not increase, and no improvement in kneading performance can be expected. When the blade thickness is less than L / D = 0.07, the blade has insufficient mechanical strength. And practicality is lost.

The screw configuration of the first kneading zone in the present invention is a combination of at least one kind of the screw parts (C) and at least one kind of the kneading disc (D). Preferably screw configuration (E)
It is provided with. By this combination, an appropriate kneading force and an appropriate resin pressure can be obtained, and the extrusion efficiency can be improved without causing trouble such as mixing of unmelted resin and vent-up.

The combination of (C) and (D) suffices if both exist, their order, the numbers of (C) and (D), the blades 3 in each screw part (C) and (D). It is sufficient that the number and the like are appropriately selected. Further, the number of kneading disks according to the configuration (E) can be appropriately selected. The composition suitable for melting and kneading by the above screw configuration is in the range of 80 to 100 parts by weight of a powdery resin, 20 to 0 parts by weight of a pellet-like resin, and 20 to 0 parts by weight of a powdery reinforcing material. is there.

In the present invention, the first kneading zone preferably has a screw configuration (F). This screw configuration (F) is a screw configuration in which one or more screw components (C) and one or more kneading discs (D) are alternately arranged in the first kneading zone. is there.

The above (F) is a specific example of the combination of the first kneading zone to which the above (F) and the above (E) are applied by repeatedly arranging the needing disk (D) and the screw part (C). Is (D) → (C) →
(D) → (C), (D) → (C) → (D) → (C) →
(E), (D) → (C) → (D) → (C) → (D),
(D) → (D) → (C) → (D) → (C) → (D) →
(E), (D) → (D) → (C) → (D) → (D) →
(C), (D) → (D) → (C) → (D) → (D) →
(C) → (E) and the like. The composition suitable for melting and kneading by the above screw configuration is in the range of 30 to 100 parts of powdery resin, 70 to 0 parts of pellet-like resin, and 70 to 0 parts of powdery reinforcing material.

The length of the screw component of the combination of the kneading disks (C) and (D) in the first kneading zone is L / D (L = length, D =
(Screw diameter) is preferably in the range of 2 to 12. If this is too small, the melting of the powdery resin tends to be insufficient, and the resin tends to vent up. Conversely, if it is too large, the resin temperature will increase, and the resin will be likely to deteriorate.

Downstream of the first kneading zone, second, third,
The same kneading zone can be provided as in the ordinary extruder. In particular, when the liquid addition nozzle 5 and the side feeder 6 as shown in FIG. 1 are provided, it is usual to provide a kneading zone on the downstream side as in the conventional case. In the second and subsequent kneading zones, reverse feed screws,
Kneading right, kneading disk (kneading left) with twist angle θ of blade 3 (see FIG. 5) of 100 to 170 degrees, neutral, wide, kneading disk with twist angle of blade 3 of less than 25 degrees, screw The part (C), the kneading disk (D), the seal ring and the like can be arbitrarily selected and used alone or in combination of two or more. Further, in the present powder extruder 1, similarly to a general extruder, a vent port 4, a liquid addition nozzle 5, and / or a side feeder 6 can be provided downstream of the first kneading zone.

One or two or more vent ports 4 can be provided, and the direction thereof may be upward or lateral, and may be either atmospheric vent or vacuum vent. At the time of liquid addition, it can be heated according to the viscosity of the liquid to be added,
Either a plunger pump or a gear pump may be used as the liquid supply pump 8 for supplying the liquid from the liquid supply tank 7. The feeders 9 and 10 are of a capacity type,
Although any of a weight type may be used, a weight type is generally preferable.

The present powder extruder 1 has an apparent specific gravity of 0.1.
It is effective for powders (powder resin, powder reinforcing material) having a particle diameter of 2 to 0.8 and / or an average particle diameter of 1 to 500 μm. Here, the apparent specific gravity refers to a value measured by a method shown in JIS K6911. The average particle diameter is a value measured by a JIS Z8801 in the case of a large particle diameter (in the case of 50 μm or more), and a value measured by a coal counter measuring instrument in the case of a small particle diameter (in a case of less than 50 μm).

The type of the powdery resin is not particularly limited.
Specific examples include polyphenylene ether, blends of polyphenylene ether and alkenyl resins, polycarbonate, polyolefin resins (high-density polyethylene, medium-density polyethylene, low-density polyethylene, linear low-density polyethylene, polypropylene, ethylene-propylene copolymer Etc.), homopolyoxymethylene, copolymer polyoxymethylene, polyphenylene sulfide, acrylonitrile / butadiene / styrene copolymer, syndiotactic polystyrene and the like. The powdered resin and pelletized resin or powdered resin may be appropriately blended and extruded. The present invention, among these,
It is effective for polyphenylene ether or a blend of polyphenylene ether and alkenyl resin.
That is, since the polyphenylene ether needs to remove volatile components contained in the polyphenylene ether, if the extrusion amount is increased, kneading is insufficient, and the volatile components increase. According to the present invention, in order to reduce the volatile content, the polyphenylene ether can be completely melted, the degassing efficiency can be improved, and the volatile content can be reduced.

Among the above, the alkenyl resin is a homopolymer or a copolymer of a vinyl aromatic compound. Examples of the vinyl aromatic compound include strain, α-methylstyrene, α-ethylstyrene, α-methylstyrene-p-methylstyrene, o-methylstyrene, m-methylstyrene and p-methylstyrene.
Each alkyl-substituted styrene such as -methylstyrene, o-chlorostyrene, m-chlorostyrene, p-chlorostyrene, p-bromostyrene, dichlorostyrene, dibromostyrene, trichlorostyrene, each halogenated styrene such as tribromostyrene, etc. Of these, styrene and α-methylstyrene are preferred.

The powdery reinforcing material to be mixed in the present invention includes heavy calcium carbonate, colloidal calcium carbonate, soft calcium carbonate, silica, kaolin, clay, titanium oxide, barium sulfate, zinc oxide, alumina, hydroxide Magnesium, talc, mica, glass flakes, hydrotalcite, needle fillers (wollastonite, potassium titanate, basic magnesium sulfate, seprite, zonotolite, aluminum borate), glass beads, silica beads, alumina beads, carbon beads , Glass balloon, metallic conductive filler, non-metallic conductive filler, carbon, magnetic filler, piezoelectric / pyroelectric filler,
They are a slidable filler, a filler for a sealing material, an ultraviolet absorbing filler, a filler for vibration damping, and a coloring agent. However, the average particle size of the needle filler is the average fiber diameter.

When the resin containing the powdery reinforcing material as described above is melted and kneaded by the present powder extruder 1 and extruded,
Other additional components can be added. For example, antioxidants, weather resistance improvers, nucleating agents for polyolefins, slip agents, various coloring agents, antistatic agents, release agents, monomer components (maleic anhydride, styrene, acrylic acid, etc.), peroxides (perhexyne) 25B, perbutyl D, perhexin 25B, etc.) can be used alone or in combination of two or more.
These may be supplied from the side feeder 6 together with the powdery reinforcing material, or may be supplied from the main hopper 1. Alternatively, one or more of fibers such as glass fiber, carbon fiber, Kepler fiber, stainless steel fiber, and copper fiber may be side-fed.

The type of pellet resin or powder resin supplied simultaneously with the powder reinforcing material is not particularly limited.
Specific examples include polyphenylene ether, blends of polyphenylene ether and alkenyl resins, polycarbonate, polyolefin resins (high-density polyethylene, medium-density polyethylene, low-density polyethylene, linear low-density polyethylene, polypropylene, ethylene-propylene copolymer Etc.), homopolyoxymethylene, copolymer polyoxymethylene, polyphenylene sulfide, polystyrene resin (polystyrene, high impact polystyrene, acrylonitrile / styrene copolymer, syndiotactic polystyrene, acrylonitrile / butadiene / styrene copolymer, etc.), Polyamide resin (nylon 6, nylon 66, etc.), polyester resin (polybutylene terephthalate, polyethylene terephthalate, etc.), styrene And the like Tajien copolymer.

The powdery resin alone or the powdery resin and the powdery reinforcing material and / or pelletized resin are charged from the main hopper 2 of the powder extruder 1 and melted and kneaded. When extruding by pressing, the temperature of the barrel is preferably set to the glass transition point Tg of the powdery resin + 30 ° C. to 350 ° C. or the melting point Tm of the powdery resin to 350 ° C. or less. If the temperature of this barrel is too low,
The state of melting and kneading of the resin tends to deteriorate, and it is difficult to improve the productivity. Conversely, if it is too high, the resin tends to deteriorate.

When the above-mentioned powdery resin or a mixture thereof is melted, kneaded and extruded by the present powder extruder 1, other additional components can be added. For example, antioxidants, weather resistance improvers, nucleating agents for polyolefins, slip agents, various coloring agents, antistatic agents, release agents, monomer components (maleic anhydride, styrene, acrylic acid, etc.), peroxides (perhexyne) 25B, perbutyl D, perhexin 25B, etc.) can be used alone or in combination of two or more.
These may be supplied from the main hopper 2 together with the powdery resin, or may be supplied from the side feeder 6.

In the present powder extruder having the side feeder 6, the materials supplied from the side feeder 6 include, for example, polystyrene, high-impact polystyrene, styrene-butadiene copolymer and hydrogenated product thereof, nylon 6, nylon 66, one or more resins such as aromatic polyamides, one or more fillers such as talc, mica, glass beads, and fibers such as glass fiber, carbon fiber, Kepler fiber, stainless steel fiber, and copper fiber Or one or more of these.

In the present powder extruder having the liquid addition nozzle 5, examples of the liquid supplied from the liquid addition nozzle 5 include mineral oil, phosphate ester, and silicon oil. Mineral oils include, for example, paraffinic, naphthenic, and aromatic oils, and phosphate esters include, for example, triphenyl phosphate, 2,2
Silicon oils such as -bis- {4- (bis (methylphenoxine) phosphoryloxy) phenyl} propane and-(3-hydroxyphenyl) diphenyl phosphate are exemplified by dimethyl silicone oil, methylphenyl silicone oil, methyl hydrogen One kind or two or more kinds can be used at the same time with silicon oil or the like.

[0056]

DESCRIPTION OF THE PREFERRED EMBODIMENTS First, the first embodiment and the first comparative example will be described.
The meanings of the symbols indicating the screws used in the kneading zone and the second kneading zone are as shown in Table 1 below. In the column of type in Table 1, "A" indicates a screw element (A), "B" indicates a screw element (B), "C" indicates a screw part (C), and "D" indicates a kneading disk (D). ), “E” means a kneading disk that can be used for the screw configuration (E).

[0057]

[Table 1]

As the extruder, a twin-screw extruder as shown in FIG. 6 (“ZSK-40” manufactured by Warner & Friedler Co., L / D = 46, 11 barrels)
An experiment was carried out by changing various screw configurations mainly in the solid transport zone and the first kneading zone. All feeders used heavy-weight feeders to minimize torque fluctuations.

Examples 1 to 16 and Comparative Examples 1 to 12
Was extruded under the following conditions unless otherwise specified. In Examples 17 to 22 and Comparative Example 13, the barrel temperature was changed as described below.

The most upstream position of the needing disk in the first kneading zone is the total length L / D of the solid conveying zone. In the case of a combination of the screw element (A) and the screw element (B), a screw element (length L / L) connecting (A) and (B) between (A) and (B).
D = 0.5). As shown in FIG. 4, the temperature of each barrel is 50 ° C. for barrel (1), 280 ° C. for barrels (2) to (5), unless otherwise specified.
(6) to (11) were set to 340 ° C. Screw rotation is 295 rpm unless otherwise specified. The vent was a vacuum vent unless otherwise specified. The pressure of the vacuum vent was 50 mmHg.

The results of Examples and Comparative Examples are summarized in Tables 4 and 5. The evaluation criteria in Tables 4 and 5 are as follows.

Judgment of vent-up: If the vent port is not closed, there is no vent-up. If the vent is blocked,
There is vent up.

Determination of unmelted material: The temperature of the press molding machine is set to P
The temperature of the PE system is set at 280 ° C. After preheating the pellets for 3 minutes,
Press for 2 minutes at a pressure of 100 kg / cm ² ,
A film having a size of × 100 mm × 100 μm was prepared, the number and size of the unmelted material were measured, and the size was scored based on the criteria in Table 2 below, and (total score) = (Σpoint) ×
Table 4 shows the result of scoring by (number) by size and number.

[0064]

[Table 2]

Torque variation: The torque variation was determined by reading the upper and lower limits of a torque recorder attached to the extruder and determining the difference between the upper and lower limits. Note that the extruder design maximum torque is 100
%.

[0066]

[Table 3]

Determination of volatile content: 1 g of the pellet was dissolved in 40 g of chloroform, and the volatile content was measured by GC-14B manufactured by Shimadzu Corporation.

Judgment of dispersion: The temperature of the press molding machine was set to PPE
The system is set at 280 ° C. After preheating the pellets for 3 minutes, 10
0kg / cm2 pressure for 2 minutes, 50mm x 1
A film of 00 mm × 100 μ was prepared, and the size of the largest lump of talc was determined. The average value of the talc maximum particle size was calculated by (vertical diameter of talc lump + width) / 2.

Example 1 Reduced viscosity 0.44, Tg = 220 ° C.
Method), a main feed of polyphenylene ether (PPE) having an apparent specific gravity of 0.694 and an average particle size of 23.1 μm, and measuring and observing the extrusion amount, torque fluctuation, presence / absence of vent-up, judgment of unmelted matter, and volatile matter, respectively. .

The solid conveying zone is composed of a screw element (A) with L / D = 7.5 (1 SC × 5) and a screw element (B) with L / D = 1.5 (2 SC × 1), and a first kneading zone. Screw configuration is R60, R40, R20, N
40 and the vent was 50 mmHg.

The extrusion rate was 85 kg / h. Operation was carried out at this extrusion rate for 1 hour, but there was no vent up, unmelted matter judgment was 77 points, torque fluctuation was ◎, volatile matter was 1010 pp
m.

Comparative Example 1 The screw element (A) having the screw structure of the solid transport zone of Example 1 was L / D = 6.0 (1 SC × 4) and the screw element (B) was L / D = 1.5 ( 2SC x 1)
The same measurement and observation were carried out in the same manner as in Example 1 except for the above.

No vent-up, unmelted matter judgment was 76
The point and the torque fluctuation were ◎ and the volatile matter was 1000 ppm, but the extrusion rate was 76 kg / h, which was smaller than that of Example 1.

Comparative Example 2 The screw configuration of the first kneading zone of Example 1 was changed to R60, R
The same measurement and observation were performed in the same manner as in Example 1 except that 40 × 2 and R20 were used.

Since the vent port was pulled with a vacuum, the semi-solid resin blocked the vent port, and the bite of the PPE powder became worse, so that the throughput decreased to 50 kg / H. As compared with Example 1, vent up, unmelted matter, and extruded amount were inferior.

Comparative Example 3 The same measurement and observation were performed on the solid transport zone of Example 1 as in Example 1 except that the screw element (B) was used instead of the screw element (A).

The throughput was 75 kg / h. Example 1
As compared with the above, the extrusion amount, especially the torque fluctuation was inferior.

Comparative Example 4 For the solid transport zone of Example 1, the length of the screw element (B) was L / D = 0, and the total length was L / D = 7.
The same measurement and observation were performed in the same manner as in Example 1 except that the value was changed to 5.

The length of the solid transport zones (A) and (B) is L
Since / D was shorter than 9, the extrusion rate was lower than in Example 1.

Comparative Example 5 For the solid transport zone of Example 1, the length L / D of the screw element (A) was set to 3.0, and the length of the screw element (B) was set to L / D = 3.0. Overall length L / D = 7.
The same measurement and observation were performed in the same manner as in Example 1 except that the value was changed to 5.

The length of the solid transfer zones (A) and (B) is L
Since / D was shorter than 9, the extrusion rate was lower than in Example 1.

Example 2 Regarding the solid transport zone of Example 1, the length of the screw element (A) was reduced from L / D = 7.5 to 4.5,
The same measurement and observation were performed as in Example 1 except that the length of the screw element (B) was set to L / D = 4.5.

The extrusion rate was increased as compared with Comparative Example 1, and the other measured values were equivalent to those of Example 1.

Example 3 For the solid transport zone of Example 1, the length of the screw element (A) was reduced from L / D = 7.5 to 4.5,
The same measurement and observation were performed as in Example 1 except that the length of the screw element (B) was changed to L / D = 6.0.

The measured values other than that in Example 1 except that the extrusion rate was increased were almost the same as those in Example 1.

Example 4 Example 1 was the same as Example 1 except that the length of the screw element (B) was set to L / D = 3.0.
The same measurement and observation were performed in the same manner as described above.

The measured values other than that in Example 1 except that the throughput was increased were almost the same as those in Example 1.

Example 5 The same measurement and observation were carried out as in Example 2 except that the target resin was a mixture of 90 parts of polyphenylene ether and 10 parts of "Asahi Kasei Polystyrene 685" under the conditions of Example 2.

The measured values other than that in Example 4 except that the extrusion rate was increased were almost the same as those in Example 4.

Example 6 The target resin was polycarbonate (PC) having a Tg of 150 ° C., an apparent specific gravity of 0.54, and an average particle size of 85 μm, which was fed as a main feed, and the barrels (2) to (11) were cooled at 230 ° C.
The same measurement and observation were performed as in Example 4, except that

The extrusion rate was 73 kg / h. After operating for 1 hour at this extrusion rate, there was no vent-up and the torque fluctuation was ◎.

Comparative Example 6 For the solid transport zone of Example 6, only the screw element (B) was used for the screw configuration, and the length L / D = 10.
The measurement and observation were performed in the same manner as in Example 6 except that the sample was set to 5.

As compared with Example 6, the extrusion amount and the torque fluctuation were inferior.

Example 7 The target resin was high-density polyethylene (HDPE) having a Tm of 131 ° C., an apparent specific gravity of 0.54, and an average particle diameter of 310 μm, which was fed as a main feed to barrels (2) to (11).
Was measured and observed in the same manner as in Example 4 except that the temperature was changed to 180 ° C.

The extrusion rate was 109 kg / h.
It was operated for 1 hour at this extrusion rate, but there was no vent up,
The torque fluctuation was ◎.

Comparative Example 7 With respect to the solid transport zone of Example 7, the screw configuration was only the screw element (B), and the length L / D = 10.
The measurement and observation were performed in the same manner as in Example 7 except that the sample was set to 5.

As compared with Example 7, the extrusion amount and the torque fluctuation were inferior.

Example 8 The procedure was performed except that the target resin was homopolyoxymethylene (POM) having a Tm of 165 ° C. and an average particle size of 300 μm, which was main-fed and the barrels (2) to (11) were set at 180 ° C. The same measurement and observation were performed as in Example 4.

The extrusion rate was 116 kg / h.
It was operated for 1 hour at this extrusion rate, but there was no vent up,
The torque fluctuation was ◎.

Comparative Example 8 Regarding the solid transfer zone of Example 8, the screw configuration was changed to the screw element (B) only, and the length L / D = 10.
The measurement and observation were performed in the same manner as in Example 8 except that the sample was set to 5.

As compared with Example 8, the extrusion amount and torque fluctuation were inferior.

Example 9 The target resin was polyphenylene sulfide (PPS) having a Tm of 275 ° C., an apparent specific gravity of 0.50, and an average particle size of 100 μm, which was fed as a main feed to barrels (2) to (11).
Was measured and observed in the same manner as in Example 4 except that the temperature was changed to 290 ° C.

The extrusion rate was 119 kg / h.
It was operated for 1 hour at this extrusion rate, but there was no vent up,
The torque fluctuation was ◎.

Comparative Example 9 Regarding the solid transport zone of Example 9, the screw configuration was changed to the screw element (B) only, and the length L / D = 10.
The measurement and observation were performed in the same manner as in Example 9 except that the sample was set to 5.

As compared with the ninth embodiment, the extrusion amount and the torque fluctuation were inferior.

Example 10 Synthetic tack polystyrene (SPS) having a Tm of 270 ° C. and an average particle size of 25 μm was used as a target resin, and the main feed was performed. The barrels (2) to (11) were set at 280 ° C. The same measurement and observation were performed as in Example 4.

The extrusion rate was 119 kg / h.
It was operated for 1 hour at this extrusion rate, but there was no vent up,
The torque fluctuation was ◎.

Comparative Example 10 For the solid transport zone of Example 10, only the screw element (B) was used and the length L / D = 1.
The measurement and observation were performed in the same manner as in Example 10 except that the value was set to 0.5.

As compared with Example 10, the extrusion amount and the torque fluctuation were inferior.

Example 11 Regarding the first kneading zone of Example 4, the screw configuration was changed to R.
The measurement and observation were performed in the same manner as in Example 4 except that the values were 60, R40, N40, and R20.

The operation was performed at an extrusion rate of 88 kg / h for 1 hour.
There was no vent-up, the unmelted material was 51 points, and the torque fluctuation was ◎. The amount of unmelted material was reduced as compared with Example 1, and the kneading performance was improved because the screw configuration (E) was employed.

Example 12 Regarding the first kneading zone of Example 4, the screw configuration was changed to R
The measurement and observation were performed in the same manner as in Example 4 except that the sample Nos. 60, R40, N40, R20, and N40 were used.

The operation was performed at an extrusion rate of 90 kg / h for 1 hour.
There was no vent-up, the unmelted material was 45 points, and the torque fluctuation was ◎. The unmelted material was reduced as compared with Example 1, and the kneading performance was improved.

Example 13 The screw configuration of the first kneading zone of Example 4 was changed to R
The measurement and observation were performed in the same manner as in Example 4 except that the sample Nos. 60, R40, N40, N40, and R20 were used.

Operation was carried out at an extrusion rate of 90 kg / h for 1 hour.
There was no vent-up, the unmelted material was 44 points, and the torque fluctuation was ◎. The unmelted material was reduced as compared with Example 1, and the kneading performance was improved.

Example 14 For the first kneading zone of Example 4, the screw configuration was changed to R
The measurement and observation were performed in the same manner as in Example 4 except that the samples were 60, R40, N40, R20, N40 and R20.

The operation was performed at an extrusion rate of 90 kg / h for 1 hour.
There was no vent-up, the unmelted material was 42 points, and the torque fluctuation was ◎. The unmelted material was reduced as compared with Example 1, and the kneading performance was improved.

In comparison with Examples 4, 11, 12, 13, and 14, when the screw configuration (E) is adopted, the kneading is improved.
Unmelted material is reduced. In addition, when two screw parts (C) are used, kneading becomes better and unmelted material is reduced.
However, when two screw parts (C) are used in succession as in Example 13, the extrusion amount tends to decrease. In Example 14, the screw configuration (E) was sandwiched between the screw parts (C) and the screw configuration (E) was employed, so that the screw configuration that was the most balanced in terms of the throughput and other measured values was compared. It can be seen that it is.

Example 15 In Example 4, the target resin was a mixture of 80 parts of polyphenylene ether and 20 parts of talc having an average particle size of 10 μm.
Example 4 except that this was supplied from the main feeder.
The measurement and observation were performed in the same manner as described above.

The operation was performed at an extrusion rate of 90 kg / h for 1 hour.
There was no vent-up, the torque fluctuation was ◎, and the talc dispersibility was a maximum average particle size of 43 μm.

Example 16 Measurement and observation were performed in the same manner as in Example 14 except that the target resin was a mixture of 80 parts of polyphenylene ether and 20 parts of talc having an average particle diameter of 10 μm, and this was supplied from the main feeder. Was done.

The operation was performed at an extrusion rate of 80 kg / h for 1 hour.
There was no vent-up, the torque variation was ◎, and the talc dispersibility was a maximum average particle size of 24 μm.

Comparative Example 11 The screw configuration of the solid transport zone of Example 15 was as follows.
Only screw element (B), length L / D = 1
The measurement and observation were performed in the same manner as in Example 15 except that the value was set to 0.5.

As compared with Example 15, the extrusion amount and the torque fluctuation were inferior, and the talc had a maximum average particle size of 45 μm.

Comparative Example 12 The first kneading zone of Example 15 was measured and observed in the same manner as in Example 15 except that the screw configuration was changed to KR60, KR40, KR40 and KR20.

Compared with Example 15, the extrusion amount and the torque fluctuation were inferior. Further, since the vent was pulled by a vacuum, the resin blocked the vent port, and the extruded amount was reduced to 50 kg / H. The dispersibility of the talc was 112 μm in the maximum average particle size.

Examples 17 to 20 and Comparative Examples 13 to 14
This is the case when there are many hard pellet-shaped resins.

In Examples 17 to 22 and Comparative Example 13 described below, the temperature of the barrels (2) to (11) was 29
It was set to 0 ° C.

Example 17 Measurement and observation were carried out in the same manner as in Example 14 except that the target resin was a mixture of 70 parts of polyphenylene ether and 30 parts of "Asahi Kasei Polystyrene 685" and supplied from the main feeder.

When the extruded amount exceeded 110 kg / H, the average torque value became 95%, so it was kept at 110 kg / H. There was no vent-up, unmelted was 51 points, and torque fluctuation was ◎.

Example 16 was the best balance among Examples 16 to 18.

Example 18 The measurement and observation were carried out in the same manner as in Example 13 except that the target powder resin was a mixture of 70 parts of polyphenylene ether and 30 parts of "Asahi Kasei Polystyrene 685" and supplied from the main feeder.

The extrusion rate was 100 kg / H. There was no vent-up, the unmelted material was 72 points, and the torque fluctuation was ◎.

Example 19 The measurement and observation were carried out in the same manner as in Example 12, except that the target powder resin was a mixture of 70 parts of polyphenylene ether and 30 parts of "Asahi Kasei Polystyrene 685" and supplied from the main feeder.

The extrusion rate was 105 kg / H. There was no vent-up, unmelted was 88 points, and torque fluctuation was ◎.

Example 20 Measurement and observation were carried out in the same manner as in Example 11 except that the target powder resin was a mixture of 70 parts of polyphenylene ether and 30 parts of "Asahi Kasei Polystyrene 685" and supplied from the main feeder.

The extruded amount was 93 kg / H. Extrusion rate 93 kg /
Lowered to H. In this state, there was no vent-up, unmelted was 106 points, and torque fluctuation was ◎.

Comparative Example 13 The screw element (B) of Comparative Example 2 was prepared by using L / D = 3.0.
The target powder resin is a mixture of 70 parts of polyphenylene ether and 30 parts of “Asahi Kasei Polystyrene 685”,
Comparative Example 2 except that this was supplied from the main feeder
The measurement and observation were performed in the same manner as described above.

The unmelted resin of polystyrene vented up and clogged the unmelted resin die, and the operation was not possible.

In Examples 17 to 20 and Comparative Example 13, since hard polystyrene was contained, compared to powder 100%,
It was easy to vent up.

Example 21 In Example 14, a side feeder was attached, and the screw configuration of the second kneading zone was changed to R40, R40, N4.
0, R20, L20 and “Asahi Kasei Polystyrene 68
5 "was supplied from a 30-part side feeder.

The amount of extrusion is controlled by the torque.
kg / H, side 36 kg / H, total output 116 kg /
It became H. No vent-up, 30 for unmelted resin
The point and the volatile content were 486 ppm.

Example 22 In Example 14, a liquid addition nozzle was attached, and the screw configuration of the second kneading zone was changed to R40, R40, N40, R2.
0, L20, a liquid addition nozzle was attached to the intermediate plate between barrels (5) and (6), and the liquid "CR741C"
30 parts by weight (manufactured by Daihachi Chemical Co., Ltd.) were added from the liquid addition nozzle.

The amount of extrusion is controlled by the torque.
kg / H, Side 30kg / H Total extrusion 120kg / H
Became. No vent-up, 28 points for unmelted resin,
Volatile content was 430 ppm.

[0145]

[Table 4]

[0146]

[Table 5]

[0147]

The present invention is as described above, and does not cause a trouble due to insufficient kneading such as mixing of unmelted resin, venting up, and removal of volatile components in the powder extrusion treatment. It is possible to stabilize the torque fluctuation, improve the extrusion efficiency, and improve the productivity of the pellet-shaped resin and the like which is performed through the extrusion.

[Brief description of the drawings]

FIG. 1 is an explanatory view schematically showing an extruder for a powdery resin according to the present invention.

FIG. 2 is an explanatory view of a screw element (A).

FIG. 3 is an explanatory view of a screw element (B).

FIG. 4 is a front view of a mixing element of a screw part (C).

FIG. 5 is an explanatory view of a kneading disk and a needing disk (D) as screw parts (C).

FIG. 6 is an explanatory diagram of an extruder used in Examples and Comparative Examples.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Extruder for powdery resin 2 Main hopper 3 Blade 4 Vent port 5 Liquid addition nozzle 6 Side feeder 7 Liquid addition tank 8 Liquid addition pump 9,10 Feeder 11 Notch

Claims (7)

[Claims] 1. A twin-screw rotary extruder, wherein a screw configuration of a solid conveying zone has an overall length of L / D = 4.5-23.
Of the following screw element (A) and the combination of the following screw element (B) having an overall length of L / D = 1.5-9, and the total of (A) and (B) The combination length is L / D = 9 to 32,
An extruder for powder, wherein the screw composition of the first kneading zone is composed of a combination of the following screw parts (C) and kneading discs (D). (A): Screw flight angle is 100 to 120 degrees and screw lead length is L / D = 0.9 to 2.0.
Screw element. (B): A screw element having a screw flight angle of 10 to 25 degrees and a screw lead length of L / D = 0.9 to 2.0. (C): One or more kinds of one or more selected from a dinging disk having a twist angle of 80 to 100 degrees, a ninging disk having a twist angle of -10 to 10 degrees, and a mixing screw in which a mountain portion of the screw is cut off. Screw parts with screw part length L / D = 0.2-2.0
Screw parts. (D): a dinging disk having a twist angle of 15 to 65 degrees and a dinging disk length of L / D = 0.4 to 2.0. 2. A powder extruder according to claim 1, wherein the screw configuration of the first kneading zone has the following screw configuration (E). (E): a screw having one or more neading disks (D) at the most downstream of the first kneading zone, the winging disks each having a thickness of L / D = 0.07 to 0.2. Constitution. 3. The powder extruder according to claim 1, wherein the screw configuration of the first kneading zone has the following screw configuration (F). (F): One or more screw parts (C) and two or more,
A screw configuration in which at least one kind of a needing disk (D) and two or more kinds are alternately arranged. 4. The extruder for powder according to claim 1, wherein the length of the screw constituting portion of the first kneading zone is in a range where L / D is 2 to 12. 5. The extruder according to claim 1, wherein one or more vent ports or vacuum vent ports are provided downstream of the first kneading zone. 6. A powder resin having an apparent specific gravity of 0.2 to 0.8 or an average particle size of 1 to 500 μm alone or a powder thereof from a main hopper of the powder extruder according to any one of claims 1 to 5. A powdery reinforcing material and / or a pellet-like resin having an apparent specific gravity of 0.2 to 0.8 or an average particle diameter of 1 to 500 μm is supplied, and the barrel temperature of the extruder is adjusted to the value of the powdery resin. An extrusion method characterized by setting the glass transition point Tg + 30 ° C. to 350 ° C. or the melting point Tm of the powdery resin to 350 ° C. and kneading and extruding. 7. The extrusion method according to claim 6, wherein the powdery resin is polyphenylene ether or a blend of polyphenylene ether and alkenyl resin.