JPH0460697B2 - - Google Patents

Description

[Detailed description of the invention]

The present invention relates to a fluid material granulation device with excellent productivity that can efficiently obtain solid particles of a desired particle size with good fluidity from a melt of an organic compound that is solid at room temperature, especially an organic rubber chemical. . "Prior Art" Various granulation methods are conventionally known as methods for granulating organic compounds such as organic rubber drugs. For example, Special Publication No. 58-10422, Special Publication No. 3210, No. 48-3210,
No. 54-62245, JP-A No. 58-74734, etc. all describe inventions in which an organic rubber chemical is dropped or dispersed in an aqueous solution containing a surfactant, a hydrophilic polymer compound, and an organic solvent, and then solidified by cooling. ing. All of these inventions are wet methods for granulation using water as a medium, and require a filtering and drying process or a solvent recovery process after granulation, and do not necessarily produce particles of a constant size and shape. It was not suitable for the purpose, required a sieving operation, and was not necessarily an excellent method from an industrial perspective. Furthermore, there was a problem in that hydrophilic polymer compounds, surfactants, etc. attached to the particles degraded the performance as organic rubber chemicals. Furthermore, JP-A-51-117738 describes a method for producing hemispherical particles by dropping a melt of a rubber anti-aging agent onto a cooled steel belt and solidifying it. It was difficult to control the amount of dripping, and productivity was also poor. On the other hand, a device for extruding fluid materials was developed in JP-A-55
-81116. The device is made of metal, and the opening or slit in the inner cylinder rotates in direct contact with the opening in the outer cylinder, so the edges of the opening are likely to wear out. There was a risk that the metal powder would mix into the organic rubber chemicals when they were taken out. In addition, if there is undissolved matter in the molten material, the undissolved matter will be caught between the opening of the outer cylinder and the opening of the inner cylinder, and as it continues to rotate, this tendency will become even stronger, causing damage and deformation of the opening. It was even dangerous. In this case, when extruding a low-melting point material such as a melt of N-alkyl-N'-phenyl-P-phenylenediamine, the size and shape of the solidified particles change, especially when used in continuous production. In many cases, the device itself or its parts must be replaced, which has the disadvantage of impeding productivity itself. "Problems to be Solved by the Invention" The present inventor has conducted extensive studies on an apparatus for efficiently and easily obtaining particles of a desired particle shape with good fluidity from organic compounds, especially organic rubber chemicals, with industrial advantage. , a granulation device consisting of a double cylindrical container is used, the part near the opening of the inner cylinder of the device is configured with a slit member removably fitted, and the diameter and wall thickness of the hole in the outer cylinder are set within a specific range. By setting these settings, it was possible to produce organic rubber drug particles of a certain size and the same shape at high speed, and the obtained organic rubber drug particles also had excellent fluidity. It has arrived. That is, an object of the present invention is to provide a granulation device with excellent productivity for efficiently producing organic compound particles having good fluidity and a desired particle size. "Structure of the Invention" The gist of the present invention is to provide an inner cylinder having an opening in the peripheral wall and capable of storing a melt of an organic compound, and an inner cylinder that is in contact with the outer peripheral surface of the inner cylinder. A double cylindrical container and an outer cylinder that rotate relative to each other and have a plurality of perforations in the peripheral wall, and the openings and perforations periodically overlap as the container rotates, allowing discharge of the molten liquid. In an organic compound granulation device consisting of a coolant kept at a temperature below the melting point of the organic compound in order to solidify the molten liquid dripping from the perforation, the part that contacts the outer cylinder near the opening is removably fitted. 1.25≧b/a≧0.60 (where a is the hole diameter and b is the wall thickness of the outer cylinder). ) An apparatus for granulating an organic compound is characterized in that it has a shape that satisfies the following. The granulation device of the present invention will be explained in detail. The granulation device of the present invention consists of a double cylindrical container,
The inner tube of the double cylindrical container has an opening penetrating its peripheral wall, and a molten liquid of an organic compound can be stored in the inner tube. Furthermore, a heat retention device or heating device is usually provided to prevent the melt from solidifying within the inner cylinder. On the other hand, the structure is such that the molten liquid of the organic compound can be continuously supplied into the inner cylinder from outside the cylindrical container through piping, and the inner cylinder is usually fixed so as not to rotate. The opening provided in the peripheral wall of the inner cylinder is usually a slit-shaped opening parallel to the central axis of the inner cylinder, and is preferably located at the lowest position of the fixed inner cylinder. By doing so, the melt can be completely discharged, and the shape of the granulated particles can also be improved. Note that the opening does not necessarily have to be parallel to the central axis, and may be oriented at a slight angle to the central axis in some cases.
Therefore, the part near the opening that comes into contact with the outer cylinder is
It is composed of a removably fitted slit member. The entire opening may be made of a slit member, or only the opening near the outer cylinder may be made of a slit member. In the former case, a large temporary opening is cut in the peripheral wall of the metal inner cylinder, and a slit member having a predetermined opening is fitted into this temporary opening. In the latter case, the peripheral wall of the metal inner cylinder near the opening is cut to a certain depth to form a recess having approximately the same external shape as the slit member, into which the slit member having a predetermined opening is fitted. Further, it is preferable that the slit member has leg portions on both long side edges thereof, and the leg portions have the advantage of ensuring secure fitting with the inner cylinder circumferential wall. When removably fitting the slit member into the inner cylinder, the slit member may be fixed or engaged with the inner cylinder so as not to move, but it is preferable that the slit member be loosely fitted. That is,
In order to eliminate the gap between the opening and the perforation, it is preferable that the slit member loosely fit into the opening and be in constant contact with the outer cylinder. Even when the slit member is loosely fitted, it is supported by the outer cylinder and does not fall off from the inner cylinder. Also, if the slit member is damaged,
By separating the outer cylinder from the inner cylinder, the slit member can be easily replaced. Although the opening of the slit member varies depending on the shape of the outer cylinder and the perforation, the length of the outer cylinder,
It can be appropriately selected according to the diameter of the perforation, and in particular, a long slit-shaped opening that matches the length of the outer cylinder and is wider than the diameter of the perforation is preferable. Further, the outer cylinder of the double cylindrical container is configured to contact the outer peripheral surface of the inner cylinder and rotate relative to the inner cylinder, and the peripheral wall of the outer cylinder is provided with a large number of regular round perforations. The structure is such that the opening of the inner cylinder and the perforation of the outer cylinder periodically overlap with each other as the cylinder rotates. These perforations are arranged in such a way as to avoid multiple perforations at once overlapping the slit opening in order to avoid or reduce pressure changes within the inner cylinder.
Preferably, they are arranged at a slight angle to the slit. Then, its wall thickness b and hole diameter a
It is necessary that the shape satisfies the general formula [] 1.25≧b/a≧0.60...[]. Further, it is preferable that the distance between the respective perforations is at least three times the diameter of the perforations between the centers of the perforations. If the value of b/a is less than 0.60, a large amount of the molten organic compound will flow out of the double cylindrical container and will not solidify easily, and interparticles may coalesce, causing the solidified particles of the organic compound to The particle size and shape are not constant, making it difficult to obtain particles of a desired size.
On the other hand, if the value of b/a is too large than 1.25, the organic compound will solidify inside the hole and will easily block the hole.
Furthermore, even if there is no clogging, the melt drains from the outer cylinder poorly, making it impossible to obtain particles with a constant particle size and shape. Furthermore, if the hole diameter a is made smaller relative to the wall thickness b, that is, if the value of b/a becomes larger than 1.25, it is necessary to reduce the rotation speed in order to obtain a good particle shape, resulting in a significant drop in productivity. result. Therefore, it is an essential requirement of the present invention that the outer cylinder wall thickness b and the perforation diameter a satisfy the relationship expressed by the general formula []. Therefore, the value of b is preferably 3 mm or less, particularly 2 mm or less, in order to make the particles of the organic compound as close to spherical as possible. By appropriately employing outer cylinders with different wall thicknesses b, particles with a desired particle size can be obtained. The granulation apparatus of the present invention will be further explained in detail using the drawings. FIG. 1 is a perspective view showing one example of the granulation device of the present invention, FIG. 2 is a partially enlarged vertical sectional view of the granulation device of FIG. 1, and FIG. FIGS. 4A and 4B are an enlarged longitudinal sectional view showing other examples of openings and perforation portions of the granulating device, and schematic perspective views of the slit member shown in FIGS. 2 and 3A, respectively. In the figure, 1 is a double cylindrical container, 2, 2', 2'' are inner tubes, 3, 3', 3'' are openings, 4, 4', 4'' are outer tubes,
5, 5', 5'' are perforations, 6, 6' are outer cylinder rotation gears,
7 is an endless steel belt, 8 is an organic compound melt supply pipe, 9, 9' is a heat retention or heating device for the melt, 10 is an organic compound particle, 11 is a stand,
12, 12', 12'' and 13, 13' are slit members, 14, 14' are slit-shaped openings, 15 is an electric motor, a is the hole diameter, b is the outer cylinder wall thickness, A is the particle diameter, and the arrow is rotation. The granulation device shown in Fig. 1 includes a coolant kept at a temperature below the melting point of the organic compound under the double cylindrical container 1;
For example, an endless steel belt 7 is disposed and moves in the direction of the arrow in conjunction with the rotation of the outer cylinder 4. The inner cylinder 2 of the double cylindrical container 1 is fixed to a stand 11 so as not to rotate, and the inner cylinder 2 has a supply pipe that supplies a melt of an organic compound to the inner cylinder and opens inside the inner cylinder 2. 8 and a heat insulating device or heating device 9, 9' arranged in the inner cylinder to prevent solidification of the molten liquid. The inner cylinder 2 has a slit-shaped opening 3 cut through the inner cylinder wall at the lowest position facing the scale belt 7, and the melt is discharged from the opening 3. As shown in FIG. 2 or 3, the details near the openings are such that the portions that contact the outer cylinder near the openings 3, 3', and 3'' are composed of slit members 12, 12', and 12''. . Looking more closely, in the case of openings 3 and 3' in Figures 2 and 3 A, openings 3 and 3'
A recess is cut in the inner cylinder peripheral wall portion near 3' that contacts the outer cylinders 4, 4' so that the slit members 13, 13' can be fitted therein.
3' is removably fitted, preferably loosely fitted. Further, in the case of the opening 3'' in Fig. 3B, a temporary opening is cut to a large size, and the slit member 12'' having the opening 3'' is fitted therein, preferably loosely fitted therein.The opening in the inner cylinder peripheral wall It is preferable that the gap (width) 3, 3' is the same size as or larger than the gap (width) of the openings 14, 14' of the slit member. A resin molded article is used.The thermosetting resin is not particularly limited, but includes, for example, phenol resin, urea resin, melamine resin, unsaturated polyester resin, epoxy resin, diallyl phthalate resin, polyurethane resin, A silicone resin or the like is used, and from the viewpoint of lubricity, abrasion resistance, and economical efficiency, a material made of phenolic resin such as Bakelite is most preferable.The outer cylinder 4 has a wall thickness b, and at least the outer circumferential surface of the inner cylinder 2 It is arranged to rotate in contact with the vicinity of the opening 3 of the cylinder, and is rotated by an external force such as an electric motor 15 through a gear 6' engaged with a gear 6 provided at the end of the outer cylinder. The outer cylinder 4 has a plurality of regularly arranged holes a that penetrate through its peripheral wall.
As the outer cylinder 4 rotates, the perforations 5 periodically overlap with the openings 3 of the inner cylinder 2, and the molten organic compound is dropped onto the steel belt 7 to cool and solidify. Organic compound particles 10 are granulated. The coolant for cooling the molten liquid constituting the granulating device is not limited to the above-mentioned steel belt 7. For example, a water tank filled with cooling water may be used, and the molten liquid may be dropped into water from the double cylindrical container 1. You may also adopt the method of In this case, since it is necessary to provide a step for separating particles and water, it is preferable to use the above-mentioned steel belt. The organic compound that can be applied to the granulation device of the present invention refers to an organic compound that is generally solid at room temperature and easily softens by heating or becomes fluid by turning into a molten liquid. Organic compounds are
Highly useful in organic rubber chemicals. The organic compound should have a melting point or softening point of 200°C or less, preferably 150°C or less, considering ease of heating and melting and workability.
The temperature is desirably below 120°C, particularly below 120°C. The melt may contain microcrystals of the organic compound that are smaller than the diameter of the perforations in the outer cylinder. Organic rubber chemicals include vulcanization accelerators, vulcanization retarders, vulcanizing agents, anti-aging agents, antioxidants, etc., but are not particularly limited to these. Specifically, the vulcanization accelerators include N-cyclohexyl-2-benzothiazolesulfenamide, N-tert-butyl-2-benzothiazolesulfenamide, 2-(morpholinothio)benzothiazole, and 2-mercaptobenzo Thiazole, benzothiazyl disulfide,
Tetramethylthiuram disulfide, tetramethyl-thiuram monosulfide, diphenylguanidine, 1,3-diphenyl-2-thiourea,
N,N'-dimethylcyclohexylamine-dibutyldithiocarbamate, 2-(2',4'-dinitrophenylthio)benzothiazole, etc. are used as vulcanization retarders, N-(cyclohexylthio)phthalimide, N-nitrosocarbamate, etc. Diphenylamine etc.
Dimorpholinodisulfide is used as a vulcanizing agent, and 1,2-dihydro-2,
2,4-trimethylquinoline polymer, octylated diphenylamine, N-phenyl-β-naphthylamine, N-phenyl-α-naphthylamine,
N,N'-diphenyl-P-phenylenediamine,
2,6-di-tert-butyl-methylphenol,
Examples include N-alkyl-N'-phenyl-P-phenylenediamine, especially N-
It is most suitable for granulating an alkyl-N'-phenyl-P-phenylenediamine anti-aging agent. N-alkyl-N'-phenyl-P-phenylenediamine having a melting point of 80 DEG C. or less usually has an alkyl group having 3 to 8 carbon atoms, including branched chains. For example, N-(1,4-dimethylpentyl)-N'-phenyl-P-phenylenediamine,
N-(1-methylhexyl)-N'-phenyl-P
-N-Secondary heptyl such as phenylenediamine-
N'-phenyl-P-phenylenediamine, N-
(1,3-dimethylbutyl)-N'-phenyl-P
-phenylenediamine, secondary hexyl such as N-(1-methylpentyl)-N'-phenyl-P-phenylenediamine, N'-phenyl-P-phenylenediamine, N-isopropyl-N'-phenyl -P-phenylenediamine and the like. Of course, the alkyl group may be a primary alkyl group. Moreover, these may be used in combination. However, it is better not to mix materials with relatively low melting points. The granulation device of the invention is particularly suitable for N-(1,4-dimethylpentyl)-N'-phenyl-P-phenylenediamine, N-(1,3-dimethylbutyl)-
N′-phenyl-P-phenylenediamine and N
-Isopropyl-N'-phenyl-P-phenylenediamine, and is most effective for N-(1,3-dimethylbutyl)-N'-phenyl-P-phenylenediamine. By the way, N-
(1,4-dimethylpentyl)-N'-phenyl-
The melting point of P-phenylenediamine is 32-34℃, N
-(1,3-dimethylbutyl)-N'-phenyl-
The melting point of P-phenylenediamine is 44-49℃, N-
The melting point of isopropyl-N'-phenyl-P-phenylenediamine is 72 to 80°C, and the other compounds mentioned above also exhibit melting points that are approximately the same as those of structurally similar compounds. Using the granulation device of the invention, e.g.
A method for granulating N-alkyl-N'-phenyl-P-phenylenediamine at temperatures below .degree. C. will be described in detail. A melt of N-alkyl-N'-phenyl-P-phenylenediamine is supplied to the inner cylinder of the apparatus of the present invention while rotating the outer cylinder, and is continuously dripped from the perforations in the outer cylinder. As a melt of N-alkyl-N'-phenyl-P-phenylenediamine, N
-Alkyl-N'-phenyl-P-phenylenediamine, or flaky or powdered N-alkyl-N'-phenyl-P-
A molten liquid obtained by heating phenylenediamine to a temperature higher than its melting point can be used as it is, or as described later, microcrystals can be precipitated in a supercooled state and used. N-alkyl-N'-phenyl-P-phenylenediamines have different melting points depending on the type, and melt viscosity also differs depending on the temperature of the melt, so each N-alkyl-N'-phenyl-P −
It is necessary to select an appropriate temperature or melt viscosity depending on the type of phenylenediamine. This can be determined by some preliminary experiments. Generally, it is preferable to supply a substance with a low melting point to a double cylindrical container at the lowest possible temperature and drop it. The melt is
Possibly because of the shearing force exerted between the outer and inner cylinders, it solidifies easily when dropped into the coolant. In the apparatus of the present invention, the solidification after dropping is quickly carried out.
Further, in order to reduce the particle size (approximately spherical shape), it is desirable that the melt be supercooled and supplied to the inner cylinder of the double cylindrical container. For example, the molten liquid is supercooled to a temperature 5 to 50° C. lower than the melting point of the refrigerant outside the granulating device.
Stirring in a supercooled state (applying shearing force) may be carried out while stirring, or may be carried out after the supercooled state has been achieved. For example, if N-alkyl-N'-phenyl-P-phenylenediamine is brought into a supercooled state while continuing to stir, fine crystals will gradually or quickly precipitate, depending on the type, and it will become a slurry. . The supercooling temperature is N-
It is appropriately determined depending on the type of alkyl-N'-phenyl-P-phenylenediamine. If the supercooled state is maintained for a long period of time, the entire melt will solidify, so once a suitable amount of crystals have precipitated, it is desirable to heat it again at a temperature above the melting point while stirring. The temperature above the melting point is sufficient if the temperature of the heating medium is above the melting point, and it is preferable that the temperature is not extremely high. For example, it is preferably higher than the melting point and within 20°C, preferably within 10°C, especially within 5°C, and the temperature of the melt itself often reaches this temperature during long-term operation. Even if the temperature of the melt itself reaches a temperature higher than its melting point, the precipitated crystals do not easily melt and remain in a slurry state. In order to perform granulation using the granulator of the present invention, the molten liquid in which the crystals of N-alkyl-N'-phenyl-P-phenylenediamine have precipitated is double-layered while it is in a slurry state. It is preferred that the coolant is supplied to a cylindrical container and kept cooled at a low temperature below its melting point, such as on an endless belt, or dropped into water. The temperature of the coolant should be as low as possible, i.e. N-alkyl-N'-phenyl-P
- The larger the difference between the melting point of phenylenediamine and the temperature of the coolant, the better. It is desirable for the content of fine crystals in the slurry to be dropped to be high, but if it is too high, there is a risk of clogging the perforations in the outer cylinder of the double cylindrical container, so the content should be 80% by weight or less, preferably 40 to 70% by weight.
It is appropriate to drop a slurry having a crystal concentration in the range of . The slurry dropped onto the coolant solidifies immediately or rapidly, and has a circular cross-sectional shape. In the granulation device of the present invention, N-alkyl-
While N'-phenyl-P-phenylenediamine is in a molten state or a slurry state, additives such as paraffin, stearic acid, zinc white, etc. can be appropriately added thereto and then granulated. To add paraffin, N-alkyl-
By a method of mixing paraffin in a heated fluidized state while N'-phenyl-P-phenylenediamine is in a melt or slurry state, and dropping a uniform mixture of the melt or slurry and paraffin onto the coolant, N-alkyl-N'-phenyl-P-phenylenediamine containing paraffin is very easily granulated. N containing paraffin
Dropping conditions for dropping the melt or slurry of -alkyl-N'-phenyl-P-phenylenediamine can be appropriately selected depending on the physical properties and content of paraffin, which can be determined by a simple test. Further, the temperature of the coolant and the crystal content in the slurry may be determined by similar tests. "Effects of the Invention" In the organic compound granulation apparatus of the present invention, the part that contacts the outer cylinder near the opening of the inner cylinder of the double cylindrical container is configured with a slit member that is removably fitted.
The perforation of the metal outer cylinder comes into contact with the opening of the inner cylinder via the thermosetting resin slit member, and direct contact between the metals is no longer performed between the opening and the perforation. Therefore, it is possible to prevent abrasion of the opening edge, as well as abrasion of the perforations, and it is possible to avoid mixing of metal powder into the organic compound particles. In addition, since the outer cylinder is in contact with the thermosetting resin slit member, the rotation of the outer cylinder is smooth, and even if the melt of the organic compound contains insoluble matter or microcrystals, opening and perforation are prevented. There is no risk of injury. Furthermore, since the thermosetting resin slit member is removably fitted to the part that contacts the outer cylinder near the opening, it can be used in the event that the slit opening or the slit member is deformed or damaged, or if the slit member is deformed or damaged. The slit member can be replaced very easily and quickly to obtain the desired particle size. Moreover, when the slit member is fitted in a loosely fitted state, even if the outer cylinder swings, it follows this movement and is always in contact with the outer cylinder, so that the molten liquid drains easily. In addition, since the part that contacts the outer cylinder is made of a slit member, even if the outer cylinder swings, the perforation always overlaps the slit opening, so the relationship between the outer cylinder wall thickness b and the perforation diameter a is Together, a uniform amount of molten liquid is dripped from the perforation. Conventionally, since a plurality of circular openings were arranged, the openings and the perforations did not overlap completely due to slight rocking of the outer cylinder, and the amount of droplets dropped also varied. Furthermore, since the granulation device of the present invention has the relationship of the general formula [ ] between the wall thickness b of the outer cylinder and the perforation diameter a, By appropriately selecting the cylinder, the particles after dropping become particles with the desired particle diameter A that exhibits a hemispherical or spherical appearance having the same shape and size, and it is possible to efficiently produce organic compound particles at high speed. . For example, when the organic compound is a melt of N-(1,3-dimethylbutyl)-N'-phenyl-P-phenylenediamine and a steel belt is used as the coolant, the outer cylinder wall thickness b and the perforation diameter a In relation to this, the following particle size A can be obtained. Wall thickness b (mm) Hole diameter a (mmφ) Particle diameter A (mmφ) 3 3 6~8 2 2 4~5 1.5 1.5 3~3.5 1 1 2~2.5 0.8 0.8 1.5~2 In other words, wall thickness, hole diameter By appropriately employing outer cylinders having different diameters, it is possible to easily obtain particles having a uniform size and shape, and having a particle diameter in the range of 1.5 mm to 10 mm, for example, as well as good liquid drainage from the slit. The particles obtained in this way are not easily crushed, are easy to measure, and do not create powder, which is extremely convenient in terms of environmental and occupational hygiene. Next, the device of the present invention will be explained in detail by way of examples.
The present invention is not limited to the following examples unless it exceeds the gist thereof. Examples 1 to 4, Comparative Examples 1 to 3 N-(1,3-dimethylbutyl)-N'-phenyl-P-phenylenediamine (melting point 44 to 49°C) in the form of flakes was heated to 60°C. and completely melted. This was gradually cooled with a refrigerant while stirring to a temperature equal to or lower than the melting point of the phenylenediamine. At 44°C, no fine crystals were observed, and when cooled to 35°C, a slurry with approximately 50% crystals precipitated was obtained. The 44°C melt and the slurry melt cooled to 35°C are continuously supplied to the double cylindrical container type granulating device shown in Figures 1, 2 and 4A. It was dropped through the perforation of the cylinder onto a steel belt cooled to 5°C. The slit member was made of Bakelite and was loosely fitted into the inner cylinder. Table 1 shows the wall thickness b of the outer cylinder, the pore diameter a, the particle diameter A of phenylenediamine, and the properties.

[Table] When the wall thickness of the outer cylinder and the perforation diameter are in the general formula [ ], the shape is spherical or nearly spherical, the size is uniform, the productivity is excellent, and the fluidity of the particles is excellent. ing. On the other hand, the value of b/a is 0.5
If the particle size is small, productivity is excellent, but the particle shape is flat and the particles have poor fluidity.
When the value of b/a is as large as 2.0, the melt does not fall regularly from the perforations and the shape is irregular, which impedes productivity. Further, when the temperature of the melt is high, the amount of the melt dripping from the perforation increases when the value of b/a is small, and the shape is more likely to be flattened than when the melt temperature is low. If the melt temperature is low and the value of b/a is large, the melt tends to solidify during perforation, making production impossible. Therefore,
It can be seen that it is necessary to drop the molten liquid kept at an appropriate temperature so that the value of b/a falls within the range of the general formula []. Further, even after the operation of Example 1 was carried out for three consecutive months, the slit-shaped opening of the Bakelite slit member in the perforated and loosely fitted state was not worn or deformed, and the thermosetting resin slit member was not worn or deformed. The condition was so good that it was incomparably better than the scratched state of the opening where the metal was not fitted and the metal directly contacted the outer cylinder. Example 2 Using a double cylindrical container type granulator having outer cylinders with a wall thickness of 2 mm and different perforation diameters a and the opening shown in FIG. The melt of the compound kept at the following temperature is
It was dropped onto an endless belt cooled to 10°C and solidified. The slit member was made of Bakelite. (1) N-phenyl-β-naphthylamine 105℃ (2) N-cyclohexyl-2-benzothiazolylsulfenamide 98℃ (3) 2,2,4-trimethyl-1,2-dihydroquinoline polymer 95℃ (Cooled to 95℃ after heating and melting at 110℃)

[Table] In the case of organic compound (1) with an outer cylinder wall thickness of 2 mm and a hole diameter of 1.5 mm, the particle size is small and shows good fluidity.
A phenomenon in which the perforations in the outer cylinder became clogged during operation occurred, and regular dripping of the molten liquid did not occur, and this tendency became stronger as the operation continued for a long time, making continuous operation impossible. Satisfactory results were obtained in all other Examples, and no deformation was observed in the openings or perforations of the thermosetting resin slit member despite long-term operation.

[Brief explanation of drawings]

FIG. 1 is a perspective view of an example of the granulation device of the present invention, FIG. 2 is a partially enlarged vertical sectional view of the granulation device of FIG. 1, and FIG. FIGS. 4A and 4B are schematic perspective views of the slit molded product shown in FIGS. 2 and 3A, respectively. In the figure, 1 is a double cylindrical container, 2, 2', 2'' are inner tubes, 3, 3', 3'' are openings, 4, 4', 4'' are outer tubes,
5, 5', 5'' are perforations, and 12, 12', 12'' are slit members, respectively.

Claims (1)

[Scope of Claims] 1. An inner cylinder having an opening in the peripheral wall and capable of storing a molten liquid of an organic compound, and an inner cylinder that rotates relative to the inner cylinder in contact with the outer peripheral surface of the inner cylinder and is attached to the peripheral wall. The double cylindrical container consists of an outer cylinder with a plurality of perforations, and as the openings and perforations periodically overlap as it rotates, allowing the discharge of the molten liquid, and the molten liquid dripping from the perforations of the outer cylinder. In an organic compound granulation device comprising a coolant kept at a temperature below the melting point of the organic compound for solidification, the part that contacts the outer cylinder near the opening is configured with a slit member detachably fitted. , and the perforation has a shape that satisfies the following general formula [] 1.25≧b/a≧0.60...[] (In the formula, a is the perforation diameter and b is the wall thickness of the outer cylinder.) An organic compound granulation device characterized by: 2. The organic compound granulation device according to claim 1, wherein the slit member is loosely fitted. 3. The organic compound granulation device according to claim 1 or 2, wherein the slit member has legs on both length edges. 4. The organic compound granulation apparatus according to claims 1 to 3, wherein the slit member is a molded article of thermosetting resin. 5. The organic compound granulation device according to claim 4, wherein the thermosetting resin is a phenolic resin. 6. The organic compound granulation device according to claim 1, wherein the organic compound is an organic rubber chemical. 7. The organic compound granulation device according to claim 1 or 6, wherein the organic compound is N-alkyl-N'-phenyl-P-phenylenediamine.