JP2003266429A - Method and apparatus for manufacturing molding material of thermosetting resin - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method and an apparatus for manufacturing a molding material which bring about fine powder very little in manufacturing the molding material and which are excellent in properties of dispersion and in uniformity of characteristics of raw materials in the molding material, and granulate the molding material continuously by simple equipment of which the equipment load is small. <P>SOLUTION: In the method for manufacturing the molding material of a thermosetting resin, the mixture of the raw materials which contains the thermosetting resin and a base material as requisite components is supplied into a space formed between an inner element and an outer element provided face-to- face with a prescribed clearance between, and it is granulated in the space by the relative rotational motions of the inner and outer elements. <P>COPYRIGHT: (C)2003,JPO

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to a method for producing a thermosetting resin molding material and an apparatus for producing the same.

[0002]

2. Description of the Related Art Thermosetting resin molding materials are usually prepared by mixing raw materials such as thermosetting resin, organic base material, inorganic base material, curing agent and release agent, and pre-kneading them with a planetary mixer or the like. After that, it is kneaded with a twin-screw extrusion kneader or a mixing roll. The molding material after kneading is usually in the form of a lump or a sheet, and in order to be used as a molding material, it is generally pulverized, classified or granulated to a certain size or smaller to be manufactured into a product.

However, when a molding material after kneading is crushed, an apparatus such as a hammer mill is usually used. In addition to being difficult to align, it was unavoidable that a large amount of fine powder was generated during crushing. If such fine powder is separated and discarded, the yield will decrease.
A method of returning to the kneading step of the molding material again using a fine powder recovery device such as a cyclone is often adopted. However, such collection and remixing of fine powder not only makes the equipment large and complicated, but also has problems such as deterioration of the working environment due to the fine powder and effects on health damage.

On the other hand, a method of granulating the thermosetting resin molding material after kneading has been partially adopted as a method of hardly generating such fine powder. As an example, by using a transfer screw device having a temperature control mechanism, the molding material after kneading is pressure-fed while maintaining a constant viscosity, a method of extruding from a screen installed in front of the device, or similarly. Examples include a method in which a molding material is pressure-fed, a screen is arranged on a side surface of a cylindrical shape, and the material is extruded by a side surface extrusion mechanism to granulate. However, in the former case, when the viscosity of the molding material is high, the transfer resistance tends to increase unless a screen with a large opening ratio is used, and on the other hand, it is difficult to give such a screen sufficient strength. Often the sex is low. In the latter case, a material retention zone may be formed depending on the structure of the side extrusion device, and it is difficult to perform stable granulation for a long time when applied to a thermosetting resin molding material. was there.

Further, in the kneading step for producing the molding material, melt kneading is carried out by applying a shearing force with a mixing roll or the like under conditions suitable for the properties of the molding material. This kneading process
It not only mixes and disperses the blended materials uniformly to make it dense, but also has the role of advancing the curing reaction of the resin halfway in consideration of workability during molding of molded products and physical properties of molded products. However, due to factors such as variations in the surface temperature of the mixing roll and instability of the supply amount of the pre-mixed product to be supplied, the dispersibility of the raw materials may become non-uniform and the characteristics of the molding materials may vary. Sometimes. There is a method of lengthening the kneading time to improve the dispersibility, but if kneading is performed for a certain time or longer, the temperature rises due to the heat supplied from the kneading device and the heat of the curing reaction of the material itself. However, there is a problem in that the curing of the material excessively progresses, or the progress of the curing partially causes the variation in the characteristics inside the material to further expand. The dispersion of the raw material components in the molding material or the variation in the curability is due to the moldability during molding,
Since it has various influences on the thermal stability and the mechanical properties of the molded product, it is necessary to minimize it. However, unlike a homogeneous system such as a liquid material, it is not easy to obtain a molding material having excellent dispersibility of raw materials by a normal kneading operation, and it may be a problem particularly in a molding material containing many base materials and the like. there were.

[0006]

SUMMARY OF THE INVENTION The present invention has been made as a result of studies for solving the problems in the conventional method for producing a thermosetting resin molding material. Provide a manufacturing method for continuously granulating a molding material and a manufacturing apparatus for the same, with extremely few occurrences, excellent dispersibility of the raw material in the molding material and uniformity of properties, and simple equipment with a small equipment load To do.

[0007]

This object is achieved by the present inventions (1) to (10) described below. (1) A method for producing a thermosetting resin molding material, in which a thermosetting resin and a base material are indispensable in a space formed between an inner core and an outer core, which are installed facing each other with a predetermined clearance. A method for producing a thermosetting resin molding material, characterized in that a raw material mixture contained as a component is supplied and granulated by relative rotational movement of the inner core and the outer core in the space. (2) The thermosetting as described in (1) above, wherein the raw material mixture is obtained by colliding raw materials with at least two kinds of components in the raw materials by impact force, crushing and / or compounding. For producing a flexible resin molding material. (3) The method for producing a thermosetting resin molding material according to (2), wherein an impact type crushing device is used as a means for causing the raw materials to collide with each other by an impact force. (4) The method for producing a thermosetting resin molding material according to the above (3), wherein a jet mill is used as the impact crushing device. (5) The raw material mixture is supplied by melting the raw material mixture and supplying it as a molten mixture.
A method for producing a thermosetting resin molding material according to any one of (4) to (4). (6) The thermosetting resin according to any one of (1) to (5) above, wherein the inner core and / or the outer core has a groove on a surface in contact with the thermosetting resin molding material. Molding material manufacturing method. (7) The method for producing a thermosetting resin molding material according to any one of (1) to (6), wherein the space has a side surface shape of a cone or a truncated cone. (8) A thermosetting resin molding material manufacturing apparatus, which is formed between an inner core and an outer core, which are relatively opposed to each other with a predetermined clearance, and which rotate relative to each other, and between the inner core and the outer core. A thermosetting resin molding material comprising a device for supplying a raw material mixture containing a thermosetting resin and a base material as essential components to a space, and a drive device for rotating the inner core and / or the outer core. Manufacturing equipment. (9) The thermosetting resin molding material manufacturing apparatus as described in (8) above, wherein an impact crushing apparatus is used for manufacturing the raw material mixture. (10) The manufacturing apparatus according to (8) or (9) above, which uses a jet mill as the impact crushing apparatus.

[0008]

BEST MODE FOR CARRYING OUT THE INVENTION The present invention will be described in detail below. The method for producing a thermosetting resin of the present invention (hereinafter, simply referred to as “production method”) is a method of producing a thermosetting resin in a space formed between an inner core and an outer core that are installed with a predetermined clearance. And a base material as essential components are supplied, and the mixture is granulated by a relative rotary motion of the inner core and the outer core in the space. Further, the manufacturing apparatus of the present invention is provided with a thermosetting resin in a space formed between an inner core and an outer core, which are relatively opposed to each other with a predetermined clearance, and which relatively rotate, and the inner core and the outer core. It is characterized by having a device for supplying a raw material mixture containing a base material as an essential component, and a drive device for rotating the inner core and / or the outer core. First, the manufacturing method of the present invention will be described in detail.

FIG. 1 is an example to which the manufacturing method of the present invention is applied. (A) is a perspective view of each of the inner core 1 and the outer core 2, and (b) is a side sectional view of a combination thereof. In the manufacturing method of the present invention, the raw material mixture is supplied to the space 3 formed between the inner core 1 and the outer core 2. 4 is an inner core surface which contacts the raw material mixture, and 5 is an outer core surface as well. Reference numeral 6 represents the clearance between the inner child and the outer child. In the example of FIG. 1, the raw material mixture 7 is supplied from one opening 8 side and is granulated in the space 3 by the relative rotational movement of the inner core 1 and the outer core 2. The molding material after granulation is discharged from the other opening 9.

In the manufacturing method of the present invention, the shape of the space formed between the inner core and the outer core is not particularly limited. For example, a conical shape, a truncated cone shape, a cylindrical shape, or a similar shape can be used. Examples include a shape along the line.
In this case, the cross section (A ₁ -A ₂ cross section in FIG. 1B) of the space has a constant thickness in any circumferential direction, except for groove portions formed on the inner and outer surfaces of the inner core, which will be described later. It has a ring shape and has a concentric circle with the center of rotation of the inner and outer cores. The thickness corresponds to the clearance between the inner core and the outer core. If necessary, a plurality of such shapes may be continuously connected to each other. These may be appropriately set depending on the shape and density of the target granulated product, the supply amount of the raw material mixture, and the like. As the space, if a frustoconical shape (see FIG. 1 (b)) of a divergent shape having a constant thickness or a conical shape is applied, the space volume in which the raw material mixture is granulated changes as the space moves to the discharge side. Since it increases, the clogging of the supplied raw material mixture is unlikely to occur, and the granulated product can be discharged smoothly in sequence, which is preferable.

In the manufacturing method of the present invention, the inner core and the outer core have a relative rotational speed difference. As a result, the shearing force acts on the supplied raw material mixture, and the mixture is twisted to be granulated. This rotation speed difference is not particularly limited, but the inner core and the outer core may be rotated in the same or opposite directions, or may be given by rotating only one of the inner core and the outer core. Among these, the method in which the outer core is fixed and the inner core is rotated is preferable because the equipment configuration can be simplified.

There is no particular limitation on the difference in the number of revolutions when granulating. This is because it largely varies depending on the composition of the raw material mixture used, the viscosity characteristics at the time of melting, the shape of the contact surface of the inner and outer cores with the raw material mixture, and the like, and the optimum range varies depending on each condition. In any case, it is preferable to give a sufficient shearing shear force to the raw material mixture, and to set it within a range such that this does not result in excessive energy supply. As an example, if a phenol resin molding material (resin content 50% by weight) using 100 mesh pass wood powder and clay is used as the base material and the clearance between the inner core and the outer core is 2 mm, it is 2
The speed is preferably 00 to 2000 rpm, more preferably 500 to 1000 rpm. This is
As the rotating inner core, a cone or a truncated cone having a vertex angle of 60 degrees and a bottom diameter of 90 mm is used, and the outer core is fixed under the granulation conditions. Generally, if this difference in rotational speed is too large, slippage occurs between the surface of the inner core and / or the outer core and the melted raw material mixture, and the frictional heat generated here causes deterioration of the raw material mixture, May affect the temperature control of. On the other hand, if the difference in the number of revolutions is too small, the raw material mixture will stay for a long time between the inner core and the outer core, so when a raw material mixture with high temperature sensitivity is used,
The desired properties may be modified by thermal history.

The clearance between the inner core and the outer core is not particularly limited, but is preferably set to 1 to 5 mm,
More preferably, it is 2 to 4 mm. This makes it possible to apply a sufficient shear shearing force to the supplied raw material mixture to granulate it, and at the same time, to prevent excess heat from being generated due to friction. Further, it is possible to obtain a granulated product having a size suitable for use as a molding material. When the clearance exceeds the upper limit value, the raw material mixture is likely to be discharged out of the apparatus before sufficient shearing shear force is applied, so that the granulation tends to be insufficient or the density of the granulated product tends to be low. is there. The size of the obtained granulated product also increases as the clearance increases. On the other hand, if the clearance is smaller than the lower limit value, a large shear shearing force will be applied during granulation, so that depending on the blending of the raw material mixture, deterioration due to heat generation or partial curing may cause clogging at the discharge site. is there.

The clearance may be constant at any portion where the inner core and the outer core face each other, or may be changed depending on the location if necessary. The clearance is preferably constant in the direction orthogonal to the transport direction of the raw material mixture, that is, in the same plane on the A ₁ -A ₂ cross section in FIG. 1B, but is appropriately set in the transport direction. be able to. For example, a large clearance is provided in the vicinity of the feed part for the raw material mixture, and the clearance is set to be gradually smaller as the discharge side of the granulated product is approached. As a result, even when a raw material mixture with a relatively low bulk density is used, it is possible to give a weak shear shear force to adjust the shape immediately after the supply under a large clearance, and gradually reduce the clearance to give a large shear shear force. Thus, it is possible to obtain a granulated product that is uniformly densified and has a small variation. Such setting is preferably performed by selecting optimum conditions according to the composition of the raw material mixture and the like.

The inner core and / or the outer core used in the manufacturing method of the present invention is not particularly limited, but preferably has a groove on the surface in contact with the raw material mixture. As a result, slippage between the raw material mixture is less likely to occur. Further, shear shearing force and compressive force can be repeatedly applied to the raw material mixture, and stable granulation can be efficiently performed. FIG. 2 (a) shows a truncated cone-shaped inner surface,
Although FIG. 2B shows an example in which the grooves 10 are formed on the outer surface of the outer surface having a shape opposite to this, the surface shape is not particularly limited to this. The cross-sectional shape of this groove is not particularly limited, but generally, one having the cross-sectional shape shown in FIG. 2C is preferably used. Figure 2
In (c), 11 is the width of the groove and 12 is the depth of the groove. This can prevent the raw material mixture from staying inside the groove. It is preferable that such a groove has a width equal to or larger than a certain width so that the material can smoothly flow in and out during the granulation process. When the cross-sectional area of the groove is small, the shear shearing force acting on the raw material mixture can be increased. On the other hand, when the cross-sectional area is large, the compressive force can be strongly applied to the raw material mixture by incorporating the raw material mixture into the groove and discharging the same repeatedly. Therefore, as in the case of setting the clearance, more preferable granulation conditions can be given by changing the size of the cross-sectional area in the granulation process.

The surface position on which the groove processing is performed is not particularly limited, and may be processed on the entire surface of the inner core and / or the outer core, or either one may be processed. Further, for example, in the vicinity of the discharge part of the granulated product, a groove of another shape is processed to control the shape of the granulated product, or groove processing is performed to make the surface of the granulated product smooth. It is also possible to provide a flat portion that does not exist.

Further, the groove processing of the inner and / or outer surface is not particularly limited, but the groove shape of the inner surface when only the inner member rotates, for example, has a shape as shown in FIG. 3, that is, a mixture of raw materials. It is preferable to have an angle with respect to the transfer direction 15. As a result, it is possible to impart the function of granulating the raw material mixture and at the same time transferring it to the discharge side. In FIG. 3, the number, angle, pitch, etc. of the grooves 13 are not particularly limited, but the grooves 13 face the inner core rotating direction 14 side from the inner raw material mixture supply side 8 toward the granulated product discharge side 9. It may be processed with an angle in such a direction. At this time, the groove on the surface of the outer core is not particularly limited, but may have a shape as shown in FIG. 2 (b), or may be processed into a shape having an angle in the opposite direction to the groove of the inner core to form the raw material mixture. The effect of transferring may be further enhanced. When the raw material mixture used in the production method of the present invention has a high temperature sensitivity, it stays in the space formed between the inner core and the outer core for a long time or causes a difference in the residence time. If so, it may affect the moldability and the properties of the cured product. By performing the groove processing on the inner core and / or the outer core, such a problem can be more reliably avoided.

In the manufacturing method of the present invention, although not particularly limited, it is preferable that the inner core and the outer core each have a temperature control mechanism. Thereby, the viscosity of the raw material mixture at the time of granulating can be optimized.
The set temperature for granulation is not particularly limited, but it is preferable to set the temperature at which granulation can be sufficiently performed and the deterioration of the molding material can be suppressed as much as possible.

The material of the surface of the inner core and the outer core used in the manufacturing method of the present invention is not particularly limited, but it is preferably one having heat resistance and wear resistance. Generally, iron, stainless steel, silicon nitride, silicon carbide, diamond and the like are preferably used. It may be appropriately selected according to the type and composition of the raw material mixture to be granulated.

In the manufacturing method of the present invention, the method of supplying the raw material mixture to the space formed between the inner core and the outer core is not particularly limited, but, for example, a conveyer conveyor, a transfer screw or the like can be used. Among these, it is preferable to use a uniaxial or biaxial transfer screw. Thereby, the supply amount can be easily adjusted, and the raw material mixture can be supplied while being pressed into the space that is the granulation site. The transfer compression ratio when using the transfer screw is not particularly limited, but is preferably set to 1.1 to 1.4. Thereby, the raw material mixture can be appropriately densified and supplied without increasing the transfer resistance. Further, it is preferable that the raw material mixture is melted and supplied as a molten mixture. As a result, the raw material mixture can be made more uniform, and the viscosity when supplied to the granulating apparatus can be made optimum and constant. The method of forming the raw material mixture as a molten mixture is not particularly limited, for example, when using a transfer screw as a method of supplying the raw material mixture, by providing a temperature control mechanism to the screw body and the casing, while transferring the raw material mixture. It can be a molten mixture. It is particularly preferable that such a temperature control mechanism can set the temperature stepwise so that the molten mixture is formed just before granulation. In addition, it is preferable that the driving device of the raw material mixture supplying device and the driving device of the granulating device can be controlled independently. As a result, the supply amount of the raw material mixture can be set to be optimum with respect to the processing capacity of the granulating device.

The raw material mixture used in the present invention contains a thermosetting resin and a base material as essential components. The thermosetting resin is not particularly limited, but phenol resin, epoxy resin, polyester resin, diallyl phthalate resin, polyimide resin and the like are used. Moreover, an organic base material or an inorganic base material is used as the base material. The organic base material includes wood powder, pulp, woven fiber, pulverized thermosetting resin cured product, and the like, and the inorganic base material includes
Examples thereof include glass fiber, aluminum hydroxide, calcium carbonate, clay, mica, silica and the like. In addition, if necessary, a curing agent, a curing accelerator, a plasticizer, a release agent, a pigment, etc. are added.

The method for producing the raw material mixture in the production method of the present invention is not particularly limited as long as it is a method in which the above raw material components are dispersed and mixed with high accuracy, but at least two or more types of components in the raw materials are A method in which the raw materials are made to collide with each other by an impact force, and crushed and / or compounded is preferable. As a result, the pulverized raw material components can be composited with other components before they are aggregated again, and a raw material mixture with high dispersion accuracy can be obtained. Examples of such a method include a method in which two or more different raw materials are simultaneously present in a fluid medium, the raw materials are caused to flow through the medium, and an impact force is applied to cause the raw materials to collide with each other. At this time, since the material converts the kinetic energy possessed by collision into collision energy and thermal energy, it is considered that pulverization, dissociation of agglomerates, surface fusion and compounding due to collision, etc. occur.

The means for colliding the raw materials with impact force is not particularly limited, but it is preferable to use an impact type crushing device. As a result, kinetic energy is efficiently given to the raw materials through the fluidized medium, and the raw materials are crushed and mixed and / or compounded by the collision between the raw materials or the collision between the raw materials and the collision target portion provided in the apparatus. can do. The impact type crushing device is not particularly limited, but may be any device capable of causing the raw materials and the medium to collide with each other at a high frequency by performing sufficient kinetic energy to perform crushing and compounding. As an example, high-pressure air is jetted from multiple nozzles arranged in the circumferential direction in a cylindrical casing to generate a high-speed swirling flow, the raw materials are supplied to the raw materials, and the raw materials collide in the high-speed swirling flow. Swirling flow powder collision type jet mill, wall collision type jet mill that collides raw materials with high pressure compressed air against a wall surface, or powder collision type counter jet mill that collides raw materials with high pressure compressed air . Counter jet mills have multiple high-pressure air nozzles arranged in an empty column-shaped device and collide the high-pressure air flow supplied from them at a single point or in a very narrow space to create a strong impact force in that space area. Is designed to have. The raw materials are usually supplied from another route and are made to exist in the apparatus, and due to the pressure difference caused by the collision of the high pressure air flow,
Raw materials are entrained in a high-pressure air stream, and the raw materials collide with each other and are crushed.

In the case of a swirling powder collision type jet mill,
Crushing and compounding are performed by colliding raw materials in a high-speed swirling flow, but since the energy of collision is not so large in principle, it is useful when it is desired to prevent excessive crushing of raw materials due to impact at the time of collision. In the case of a wall collision type jet mill, the raw materials collide with the medium on the equipment wall surface and are crushed, and when they remain on the wall surface, the next material collides with them to form a composite material, which has a relatively high adhesive property. Application to small raw materials is preferred. In the case of the counter jet mill, since the raw materials almost directly collide with each other via the medium, the energy given to the raw materials is large.
Therefore, it is particularly useful when high energy is required for crushing or compounding.

The thermosetting resin molding material contains a thermosetting resin, a base material, a curing agent and a curing aid.
Each of these components has a different function. For example, the thermosetting resin determines the basic physical properties of the molding material and acts as a binder in the molding material.
The base material is compounded mainly for the purpose of imparting mechanical properties and electrical properties. Then, a curing agent and a curing aid are mixed in order to accelerate the curing reaction of the thermosetting resin. Therefore,
In order to effectively exhibit the function of each component, these raw material components are preferably dispersed as uniformly as possible.

In the conventional method for producing a thermosetting resin molding material, the raw material mixture which has been roughly mixed is melt-kneaded by a twin-screw extrusion kneader or a mixing roll to disperse and mix the raw material components. The production method of the present invention is characterized in that the step of applying such a large shearing force to the raw material mixture is not performed. Therefore, it is preferable that the raw material mixture is mixed with high accuracy at the time of supplying to the granulating device. In the production method of the present invention, the thermosetting resin molding material contains the thermosetting resin and the base material as essential components, but these are often solid materials having a certain particle size. Usually, when a plurality of types of solid components are dispersed and mixed, it is general that each component is pulverized into fine particles and then mixed. However, finely divided raw materials often cause strong secondary aggregation due to electrostatic force acting between the particles. Since dissociation of secondary agglomeration requires a very large amount of energy, even if the raw materials that have undergone secondary agglomeration are simply mixed or subjected to mechanochemical treatment, mixing or Only compounding occurs. Therefore, there is a limit to the mixing accuracy of different components. On the other hand, in the manufacturing method of the present invention, preferably different raw materials are made to collide with each other by an impact force. The raw materials are crushed by the energy of collision and at the same time complexed by collision with other components. That is, the finely pulverized raw material can be mixed and / or made into composite particles with another raw material without being aggregated again, and different raw materials can be dispersed and mixed with higher accuracy.

When obtaining the raw material mixture, various auxiliary treatments can be combined with the method of the present invention. For example, each raw material may be subjected to pretreatment such as pulverization, classification, shape control, humidity control, drying, and chemical treatment so as to be suitable for pulverization and / or compounding. Further, in order to efficiently obtain composite particles in a multi-component system, some or all of the materials are mixed in advance with a Henschel mixer or the like, or the equipment that can give mechanochemical action is used It may be processed after preliminary fusion.

Next, the manufacturing apparatus of the present invention will be described. A specific example of the manufacturing apparatus of the present invention will be described with reference to FIG. FIG. 4 (a) is a schematic view of an impact type crushing apparatus for producing a raw material mixture, and FIG. 4 (b) is a schematic view of a combination of an apparatus for melting a raw material mixture and supplying it as a molten mixture and an apparatus for granulating. First, FIG. 4A will be described. Raw material components are 10 ~ 500μ
The coarsely pulverized product having a size of m is pre-mixed with a Henschel mixer or the like to obtain a mixture 15, which is a hopper 16
I will stock it. A stirring device 17 is used as necessary to prevent the occurrence of bridges inside the hopper. Mixture 1
6 is sequentially supplied in a fixed amount by the rotary valve 18, and is supplied to the jet mill main body 19 from the position of the upper portion 20 of the jet mill main body. The mixture 16 is supplied with a high-speed jet stream by the air nozzles 21 (two locations are shown in the drawing, but the number is not limited to this and may be more than two locations) in the jet mill to repeatedly collide with each other and atomize. Alternatively, after being made into fine particles and made into a composite, it is discharged from the upper part of the jet mill by the air suction 25 to the pipe 22, and sent to the mixture storing part 24 via the cyclone 23. Figure 4 (a)
In the above, the case where the raw material mixture thus obtained is captured by a cyclone has been described as an example, but the raw material mixture can be continuously supplied as it is to a granulating device described later. Next, FIG. 4B will be described. The raw material mixture produced by the method shown in FIG. A stirring device 27 is used as necessary to prevent the occurrence of bridges inside the hopper. The raw material mixture is sent by a transfer screw 28 to a granulating device including an inner core 1 and an outer core 2. Although not shown, the transfer screw 28 and the casing 29 are at a normal temperature just below the hopper 26, but the raw material mixture is gradually heated and melted shortly before being supplied to the granulating device. The temperature is controlled so that A compression ratio is set in the transfer screw, and the raw material mixture is transferred, heated and softened, densified, and supplied to the space formed between the inner core 1 and the outer core 2. Although not shown, the inner core and the outer core are each grooved on the surface in contact with the material, and the material is granulated by the repeated shearing and compressive forces in the space.

[0029]

EXAMPLES The effects of the present invention will be described below based on examples.

1. Raw materials The following raw materials were used (content is% by weight based on the whole). 1) Thermosetting resin: Novolac type phenolic resin 45%
(“A-1082” manufactured by Sumitomo Akita Bakelite: average particle size 60 μm) 2) Curing agent: hexamethylenetetramine 5% (average particle size 100 μm) 3) Curing aid: calcium hydroxide 1% (average particle size 13 μm
m) 4) Organic base material: Wood powder 31% (100 mesh passing product) 5) Inorganic base material: Clay 15% ("N manufactured by Tsuchiya Kaolin Industry"
N Kaolin clay ": 100 mesh passed product) 6) Pigment: carbon black 1.5% (average particle size 100)
μm) 7) Release agent: Stearic acid 1.5% (average particle size 100μ
m)

2. Preparation of raw material mixture Pre-mix the above raw materials with a Henschel mixer (1 min /
1800 rpm), and then a powder collision type jet mill (Hosokawa Micron Co., Ltd. counter jet mill 200AF
G, nozzle diameter 3mm x 3), air pressure 600k
The raw material mixture was obtained by treating with Pa and a compressed air amount of 1.7 m ³ / min.

3. Production of Molding Material << Example 1 >> The raw material mixture was placed in the equipment shown in FIG. 4 (the inner core and the outer core are those shown in FIG. 1B) and treated under the following conditions. (1) Transfer screw size specification: uniaxial type, outer diameter 20 mm, compression ratio = 1.3 Set temperature of screw body and casing: Raw material mixture is equally divided into 3 sections from feeding of raw material mixture to granulator inlet. The charging part was 25 ° C., the intermediate part was 40 ° C., and the granulator side was 100 ° C. Rotation speed: 40 rpm (2) Inner shape: frusto-conical dimension specifications: short diameter side (material supply side) outer diameter 30 mm, long diameter side (granulation product discharge side) outer diameter 90 mm, frustoconical height 82 m
m Groove shape: As the groove shape, one having the cross-sectional shape shown in FIG. 2 (c) and the plane shape shown in FIG. 3 was used. The cross section of the groove had a width of 4 mm and a depth of 2 mm, and 12 grooves were processed at a uniform pitch. Operating conditions: Used by driving. Rotation speed is 800r
pm. Temperature control setting: 50 ° C. (3) Outer shape: A shape having the same clearance in all parts facing the inner cone which is a truncated cone shape. Clearance: 2.0 mm. Groove shape: the plane shape shown in FIG. 2B and FIG.
The cross-sectional shape shown in (c) was used, and the cross-section width, depth, and number of grooves were the same as those of the one processed on the inner core side. Operating conditions: Fixed and used. Temperature control setting: 50 ℃

<< Example 2 >> The rotation speed of the inner core was 300 rpm.
The conditions were the same as in Example 1 except that the above was set. << Example 3 >> The process was performed under the same conditions as in Example 1 except that the rotation speed of the inner core was set to 1500 rpm. << Example 4 >> The process was performed under the same conditions as in Example 1 except that the clearance was set to 4.0 mm. << Example 5 >> The process was performed under the same conditions as in Example 1 except that the clearance was set to 1.0 mm. << Example 6 >> The process was performed under the same conditions as in Example 1 except that the clearance was set to 6.0 mm.

Comparative Example 1 The same raw material mixture as in Example 1 was kneaded with a kneading roll at 90 ° C. for 3 minutes, cooled, coarsely crushed with a hammer mill, and then crushed with a cutter mill to obtain a phenol resin having an average particle diameter of 2 mm. A molding material was obtained.

4. Evaluation The following items were evaluated using the molding materials obtained by the methods of the above Examples and Comparative Examples. In addition, molding of samples for general property evaluation of these molded products was performed under the following conditions. (Molding conditions) Molding method: Injection molding Temperature: 175 ° C. Injection pressure: Effective pressure 1200 kg / cm ² Curing time: 60 seconds

The evaluation items and the test conditions are as follows. (1) Material Fine powder amount: For Examples 1 to 6, after granulation, Comparative Example 1
For 100 g, each 100 g of the crushed molding material was sampled, and an 80 mesh sieve (flat tatami woven wire mesh) for the whole
The passing amount (% by weight) was measured. Average particle size: For Examples 1 to 6, the maximum diameter in the cross-section of the center of the major axis of 100 obtained granules was measured and the average value was obtained. For Comparative Example 1, the maximum unidirectional diameter was measured for 100 crushed products, and the average value was calculated. Apparent Density: 200 g of each molding material after granulation for Examples 1 to 6 and after crushing for Comparative Example 1 was sampled, and the apparent volume was measured to calculate the apparent density.

(2) Molded product  Bending strength of molded products: JIS K6911  Insulation resistance: JIS K6911

[0038]

[Table 1]

From the results shown in Table 1, in Examples 1 to 6 to which the granulation method of the present invention was applied, the amount of fine powder was compared with that in the case of being manufactured by the conventional method without affecting the general characteristics of the molded product. It was confirmed that a granulated product with a very small particle size was obtained, and that materials with different particle sizes could be obtained by changing the clearance between the inner core and the outer core. In addition, although the number of rotations of the inner core was changed, no substantial difference was observed in the characteristics of the obtained granulated product or the cured product using the same, and when using the production method of the present invention, the operating condition It turned out that the target material can be obtained in a wide range.

[0040]

INDUSTRIAL APPLICABILITY The present invention provides a raw material mixture containing a thermosetting resin and a base material as essential components in a space formed between an inner core and an outer core, which are installed to face each other with a predetermined clearance. A method for producing a thermosetting resin molding material, which comprises supplying and granulating by a relative rotational motion of the inner core and the outer core in the space, without affecting the characteristics of the cured product. Using a simple and compact equipment, it is possible to continuously and efficiently obtain a granulated product with less generation of fine powder. Therefore, the present invention is useful as an industrial method for obtaining a granulated molding material without using large equipment.

[Brief description of drawings]

FIG. 1 is an example in which the manufacturing method of the present invention is applied.
Is a perspective view and (b) is a side sectional view.

FIG. 2 is an example of a groove shape in the manufacturing method of the present invention,
(A) is a plane shape of the inner child surface (side sectional view), (b) is a plane shape of the outer child surface (side sectional view), (c) is a cross sectional shape of (a) and (b).

FIG. 3 is an example of a groove shape in the manufacturing method of the present invention,
Plane shape of the inner core surface (side sectional view).

FIG. 4 is an example of a manufacturing apparatus (side sectional view) to which the manufacturing method of the present invention is applied.

[Explanation of symbols]

1 Uchiko 2 Gaiko 3 Space formed between inner child and outer child 6 Clearance between inner child and outer child 7 Raw material mixture 10 Grooves machined on the inner core surface 11 Groove width 12 Groove depth 13 Grooves machined on the inner core surface 14 Inner rotation direction 16 Raw materials 20 Impact type crusher body 24 cyclone 28 Transfer screw

Continued front page    F term (reference) 4F201 AA36 AP01 BA02 BC19 BK06                       BK13 BK71 BL33 BN18 BN29                       BQ10

Claims (10)

[Claims] 1. A method for producing a thermosetting resin molding material, wherein a thermosetting resin and a base material are provided in a space formed between an inner core and an outer core, which are installed facing each other with a predetermined clearance. Supply a raw material mixture containing as an essential component,
A method for producing a thermosetting resin molding material, characterized in that granulation is performed by relative rotational movement of the inner core and the outer core in the space. 2. The heat according to claim 1, wherein the raw material mixture is obtained by crushing and / or compounding at least two kinds of components in the raw materials by colliding the raw materials with impact force. A method for producing a curable resin molding material. 3. The method for producing a thermosetting resin molding material according to claim 2, wherein an impact-type crushing device is used as a means for causing the raw materials to collide with each other by an impact force. 4. The method for producing a thermosetting resin molding material according to claim 3, wherein a jet mill is used as the impact crushing device. 5. The method for producing a thermosetting resin molding material according to claim 1, wherein the raw material mixture is supplied by melting the raw material mixture and supplying it as a molten mixture. 6. The thermosetting resin molding according to claim 1, wherein the inner core and / or the outer core has a groove on a surface in contact with the thermosetting resin molding material. Material manufacturing method. 7. The method for producing a thermosetting resin molding material according to claim 1, wherein the space has a side surface shape of a cone or a truncated cone. 8. A thermosetting resin molding material manufacturing apparatus, wherein the thermosetting resin molding material manufacturing apparatuses are installed to face each other with a predetermined clearance.
A device for supplying a raw material mixture containing a thermosetting resin and a substrate as essential components to a space formed between the inner core and the outer core, the inner core and the outer core, which relatively rotate, and the inner core and the outer core. And / or a device for manufacturing a thermosetting resin molding material, which has a drive device for rotating an outer member. 9. The thermosetting resin molding material manufacturing apparatus according to claim 8, wherein an impact crushing apparatus is used for manufacturing the raw material mixture. 10. The manufacturing apparatus according to claim 8 or 9, wherein a jet mill is used as the impact type crushing apparatus.