JP2005041967A - Manufacturing process of carbon black for blend in composition and thermosetting resin composition - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a manufacturing process of carbon black for blend in compositions the aggregate of which is efficiently dispersed and not liable to re-aggregate and a thermosetting resin composition blended with the carbon black. <P>SOLUTION: The manufacturing process of carbon black for blend in compositions comprises dispersing carbon black with an impact crusher and coating the surface of the carbon black with a coupling agent. The thermosetting resin composition contains a thermosetting resin, an inorganic filler and the carbon black for blend in compositions obtained by the manufacturing process. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

【００５３】
＜表の注＞
（１）エポキシ樹脂：ジャパンエポキシレジン社製・「ＹＸ４０００Ｈ」（ビフェニル型エポキシ樹脂、融点１０５℃、エポキシ当量１９５ｇ／ｅｑ）
（２）硬化剤：ノボラック型フェノール樹脂（軟化点６５℃、水酸基当量１０４）
【００５４】
実施例１及び２は、カーボンブラックを衝撃式粉砕装置で分散処理した後、カップリング剤によりその表面を被覆処理する本発明の製造方法により得られたカーボンブラックであり、未処理のカーボンブラックを使用した比較例と比べて、平均粒子径が小さく分散性に優れたものであった。
【００５５】
【発明の効果】
本発明は、カーボンブラックを衝撃式粉砕装置で分散処理した後、カップリング剤によりその表面を被覆処理することを特徴とする組成物配合用カーボンブラックの製造方法であり、凝集性の強いカーボンブラックを効果的に分散させることができるとともに、再凝集をも抑えることができる。本発明の組成物配合用カーボンブラックの製造方法により得られたカーボンブラックは例えば、高い絶縁性能が要求される電子部品封止用の熱硬化性樹脂組成物材などに、特に好適に用いることができるものである。
【図面の簡単な説明】
【図１】（ａ）カーボンブラックの供給装置（側断面図）
（ｂ）カップリング剤の供給装置（側断面図）
【図２】カーボンブラックの表面を、カップリング剤により被覆処理する装置の一例（側断面図）
【図３】（ａ）ずり剪断力を与える装置の内子表面の溝形状（側面図）
（ｂ）ずり剪断力を与える装置の内子表面の溝形状（断面図）
【符号の説明】
１ カーボンブラック
５ スプレー装置
１１ カップリング剤
１３ ノズル霧化装置
２１ 混合装置
３１ ずり剪断力を与える装置[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a composition-containing carbon black and a thermosetting resin composition obtained by blending the method.
[0002]
[Prior art]
Carbon black is a fine particle produced by supplying raw oil such as natural gas or creosote oil to a high-temperature furnace in the form of a spray or vapor and is added to a rubber material to reinforce mechanical strength. It is used as a colorant in general printing inks and paints. Moreover, it may be used for imparting a specific function to a resin composition such as a molding material and a sealing material in addition to a colorant.
[0003]
One of the resin compositions containing the carbon black is a thermosetting resin composition used for sealing electronic components such as diodes, transistors, and integrated circuits (ICs). For example, an epoxy resin composition having excellent electrical characteristics and moisture resistance is used for sealing integrated circuit components.
[0004]
In such a thermosetting resin composition, the above-described carbon black is used as a colorant or for imparting a printing property to a specific laser. Carbon black can impart such an effect with a small amount of blending.
However, in recent years, with the increase in integration density of integrated circuits, the size and thickness of packages have been reduced along with the increase in size of semiconductor chips. As a result, the fine pitches of packages have progressed, and the number of packages with narrow pitches between inner leads and wires has increased.
[0005]
The average particle size of carbon black single particles is usually 100 nm or less, but rarely exists in the state of such single particles, and usually a primary aggregate of a chain structure called a structure is formed by chemical bonding. It is known to form. Since the binding force of this primary aggregate is very strong, it is considered that the substantial minimum dispersion diameter of carbon black is a structural unit.
The size of the primary aggregate is usually 1 μm or less, but carbon black further forms secondary aggregates and tertiary aggregates due to physical bonds of the primary aggregates. This size may grow to several μm to several hundred μm, or even larger. For this reason, if there is a large amount of such aggregates between leads or gold wires in a fine pitch package, the insulation of the package due to leakage or short circuit due to the conductivity of carbon black. There was a problem that reliability decreased.
[0006]
To solve such problems, for example, agitation energy is applied to a mixture of an inorganic filler and carbon black blended in the thermosetting resin composition, and the carbon black aggregate is dispersed to a certain size in advance. After that, there is a method of obtaining a thermosetting resin composition by mixing with other components (for example, see Patent Document 1). Or there exists the method of melt-mixing the resin component and carbon black to mix | blend beforehand, and mixing with another component after this and obtaining a thermosetting resin composition (for example, refer patent document 2).
Although the above method can obtain a certain effect, the effect of dispersing the aggregate may not be sufficient depending on the use.
[0007]
[Patent Document 1]
JP 2000-169676 A
[Patent Document 2]
JP 2003-026903 A
[0008]
[Problems to be solved by the invention]
The present invention relates to a method for producing a carbon black for blending a composition that can effectively disperse aggregates and is less likely to aggregate again, and a thermosetting resin composition that blends the carbon black. Is to provide.
[0009]
[Means for Solving the Problems]
Such an object is achieved by the following present inventions (1) to (4).
(1) A method for producing a carbon black for blending a composition, wherein the surface of the carbon black is subjected to a dispersion treatment with an impact pulverizer and then the surface thereof is coated with a coupling agent.
(2) Carbon black for composition blending, in which carbon black is dispersed with an impact pulverizer and then coated with a coupling agent, and then further dispersed with an impact pulverizer Manufacturing method.
(3) The method for producing carbon black for blending a composition according to the above (1) or (2), wherein the impact pulverizer is a jet mill.
(4) A thermosetting comprising a thermosetting resin, an inorganic filler, and a carbon black for blending a composition obtained by the production method according to any one of (1) to (3). Resin composition.
[0010]
DETAILED DESCRIPTION OF THE INVENTION
Below, the manufacturing method of the carbon black for a composition mixing | blending of this invention and a thermosetting resin composition formed by mix | blending this are demonstrated.
The method for producing a carbon black for blending a composition according to the present invention is characterized in that carbon black is subjected to a dispersion treatment with an impact pulverizer and then the surface thereof is coated with a coupling agent.
The thermosetting resin composition of the present invention is characterized by containing a thermosetting resin, an inorganic filler, and a carbon black for blending a composition obtained by the production method of the present invention.
First, a method for producing a carbon black for blending a composition of the present invention will be described.
[0011]
In the method for producing carbon black for blending a composition of the present invention (hereinafter sometimes simply referred to as “production method”), carbon black is dispersed with an impact pulverizer and then the surface is coated with a coupling agent. It is characterized by doing. As a result, the aggregate of carbon black can be made substantially smaller than a certain particle size, and re-aggregation of the carbon black can be suppressed.
In the present invention, “dispersion treatment” refers to an operation of unraveling the aggregates (structures) of carbon black forming secondary or tertiary aggregates.
[0012]
The impact pulverizer used here is not particularly limited, and examples thereof include jet mills such as a swirling powder collision type jet mill and a powder collision type counter jet mill.
A jet mill is an apparatus that makes solid materials collide with each other by a high-speed jet flow using air or the like as a medium. When carbon black is dispersed using such an apparatus, aggregates can be dispersed by collision of carbon black particles.
[0013]
After the carbon black is dispersed by this impact pulverizer, the surface is coated with a coupling agent. Thereby, it can suppress that the carbon black particle disperse-processed with the impact-type grinding | pulverization apparatus forms an aggregate again by influences, such as moisture absorption.
[0014]
Although it does not specifically limit as a coupling agent used here, An aminosilane coupling agent, an epoxysilane coupling agent, a mercaptosilane coupling agent, etc. can be used. These may be used alone or in combination of two or more.
In addition, as a coupling agent here, what is in the form of a liquid may be used as it is, what diluted this with the organic solvent etc., or what melt | dissolved the thing of the solid form in the organic solvent etc. Can also be used.
[0015]
The method of coating the surface of carbon black with the above coupling agent is not particularly limited. For example, a method of spraying a coupling agent on carbon black, after kneading carbon black in a coupling agent diluted with an organic solvent And a method of removing the organic solvent.
[0016]
In the production method of the present invention, as a method of coating the surface of carbon black with a coupling agent, the carbon black and the coupling agent are brought into contact with each other in a flowing state, whereby the surface of the carbon black is cupped. It is preferable to use a method of attaching a ring agent.
[0017]
In this method, first, for example, carbon black after the dispersion treatment is supplied into a device having a cylindrical closed space using a spray device such as a spray device or an injection device, and the carbon black flows in the device. State.
As a result, sufficient kinetic energy can be given to the carbon black, and even if an aggregate is being formed, it has the effect of dissociating the carbon black particles. It can be flowed into the device.
When supplying the carbon black after the dispersion treatment into the apparatus, the direction is not particularly limited, but it is preferable that the carbon black forms a swirl flow in the cylindrical treatment space and flows for a long time. .
[0018]
Next, the coupling agent that has been atomized by a nozzle atomizer or the like is sprayed onto the moving carbon black. Thereby, both can contact in the state which flowed and can make a coupling agent adhere to the surface of carbon black.
By such a method, even when the amount of the coupling agent with respect to the carbon black is small, the supply amount of both can be controlled and brought into contact with high accuracy, and the mutual wettability is usually not so good and simple. Even when it is difficult to mix the carbon black, the surface of carbon black can be coated with a coupling agent with high uniformity.
[0019]
Next, an apparatus to which such a method is applied will be described with reference to the drawings.
This apparatus has an apparatus for supplying carbon black, an apparatus for supplying a coupling agent, and a mixing apparatus for bringing the carbon black and the coupling agent into contact with each other while being moved.
FIG. 2 shows an example of such an apparatus, in which carbon black is supplied from a spray apparatus, and a swirling flow is applied in the mixing apparatus to flow, and a coupling agent finely divided by a nozzle spray apparatus is supplied thereto, Both are brought into contact with each other, and the surface of the carbon black is coated with a coupling agent.
[0020]
In FIG. 1, (a) is an apparatus for supplying carbon black, and (b) is a side sectional view of an apparatus for supplying a coupling agent.
In FIG. 1 (a), the carbon black 1 can be stocked in the hopper 2. In order to prevent the occurrence of bridging of the carbon black 1 inside the hopper 2, a stirring device 3 can be used as necessary. Carbon black 1 is sequentially supplied in a fixed amount by a rotary valve 4 in accordance with the mixing ratio with the coupling agent, and supplied to a mixing device by a spray device 5. The compressed air supply device 6 is used for supplying the carbon black 1.
Further, in FIG. 1B, the coupling agent 11 is sequentially supplied by a liquid feed pump 12 that supplies a constant amount thereof, and is supplied to a mixing device by a nozzle atomizing device 13. The compressed air supply device 14 is used to supply the coupling agent 11.
[0021]
FIG. 2 is a cross-sectional side view of a mixing device that makes contact between the carbon black 1 and the coupling agent 11 and a mixture recovery device.
In FIG. 2, the carbon black 1 is supplied from the supply unit 22 into the mixing device 21. Here, the mixing device 21 has a shape in which a cylinder and a truncated cone are combined. After the carbon black 1 is supplied into the mixing device 21 in the tangential direction of the cross section, the swirl flow 24 is given to the mixing device 21. It goes down while turning inside. On the other hand, the coupling agent 11 is sprayed from the supply unit 23 toward the center in the mixing device 21, and a part of the coupling agent 11 comes into contact with the carbon black 1 at the time of spraying. The two materials can be contacted during the flow.
[0022]
The treated material 25 obtained in this way can be used as it is, but FIG. 2 further includes a device for applying a shearing shear force to the treated material 25. Thereby, the adhesion of the coupling agent 11 to the carbon black 1 can be made stronger.
[0023]
In FIG. 2, the processed material 25 is sent from the lower part of the mixing device 21 to a device 31 that applies a shear shear force. The device 31 for applying a shearing shear force includes an inner core 32 and outer cores 33 and 33 ′. The inner core 32 has a truncated cone shape, and the outer cores 33 and 33 ′ have a certain clearance with respect to the inner core 32. This is a shape that confronts each other. The clearance can be set to an optimal value as appropriate depending on the size of the apparatus, the processing amount, and the like.
The mixed material 25 is supplied to a space 34 formed between the inner core 32 and the outer cores 33 and 33 ′, where shear shear is caused by relative rotation between the inner core 32 and the outer cores 33 and 33 ′. Powered. Although not shown, the inner core 32 and the outer cores 33 and 33 ′ each have a temperature control device that can be set independently, and the inner core 32 has a surface in contact with the mixed material 25. Grooving is applied. The inner core 32 has a driving device 35 and rotates. The outer cores 33 and 33 'have fixed specifications. The treated material 25 is subjected to a shear shear force in the space 34 and then stored in the recovery device 36. The cyclone device 37 is for discharging the air supplied into the mixing device 21 when the carbon black 1 and the coupling agent 11 are supplied.
[0024]
FIG. 3 shows the shape of the groove formed on the inner core 32 used in the device 31 for applying the shearing shear force. FIG. 3A shows the processed shape of the groove on the surface of the inner core 32, and FIG. 3B shows the sectional shape of the groove.
In FIG. 3A, the groove 32 a on the surface of the inner core 32 has an angle with respect to the introduction direction 53 of the material 25 after processing, and is processed in a curved shape toward the rotation direction 54 side of the inner core 32. Thereby, not only the shearing force is given to the mixed material 25 but also a function of sequentially discharging it.
FIG. 3B shows a cross-sectional shape of the groove 32a. Here, the groove width 32b and the groove depth 32c can be appropriately optimized depending on the size of the apparatus, the processing amount, and the like.
2 and 3 show an example in which the groove 32a is processed only in the inner core 32. In addition to this, the groove processing is performed on the surface in contact with the material 25 after the processing of the outer cores 33 and 33 ′. It can also be used in combination.
[0025]
The carbon black thus obtained has its surface coated with a coupling agent in a state in which the particle size when dispersed by an impact pulverizer is substantially maintained.
Carbon black after such a treatment reduces the particle size of carbon black and improves self-fluidity, so that when blended in various compositions, the mixing accuracy in the composition can be improved. it can.
In addition, since it is possible to suppress re-aggregation to form an aggregate having a large particle size, for example, even when blended in a thermosetting resin composition and used for sealing a semiconductor package, the insulation characteristics due to the aggregate A decrease can be prevented.
[0026]
The coating treatment of the carbon black surface with the above coupling agent is preferably performed after the aggregate is dispersed by an impact pulverizer and before being affected by moisture absorption or the like as much as possible.
[0027]
The above-mentioned effects can be obtained if the coating with the coupling agent is performed on at least a part of the surface of the carbon black particles, but it is preferable that substantially the entire surface is coated. Thereby, the higher effect described above can be obtained.
[0028]
The production method of the present invention is not particularly limited, but the carbon black particles obtained by the above method can be further subjected to dispersion treatment with an impact pulverizer.
Thereby, the particle size of the carbon black particles can be further reduced. Further, even when the coupling agent is localized on the carbon black in the state after the coupling agent treatment, it is considered that there is an effect of averaging this.
Further, after the dispersion treatment is again performed by the impact pulverizer, the particle size can be substantially maintained. The reason for this is that when the carbon black particles after the surface is coated with the coupling agent are dispersed, the portion where the surface is not coated with the coupling agent is exposed, but there are many portions where the surface is not coated in this way. This is because bonding to form an aggregate is considered to be extremely small in terms of probability.
[0029]
Some carbon black particles have various characteristics depending on the production method, etc., but in particular, when using those that easily form aggregates or those that are difficult to disperse aggregates, or when blended into a composition, carbon black particles When it is desired to reduce the particle size of the particles, it is effective to perform the dispersion treatment again after the coating treatment with the coupling agent.
In addition, the dispersion | distribution process implemented after the coating process by a coupling agent may be performed once, and can also be performed in multiple times.
[0030]
In the method for producing the composition of the present invention, the particle size of the carbon black particles obtained by the above method depends on the type of carbon black, the type and operating conditions of the impact pulverizer, the degree of surface coating treatment with a coupling agent, etc. Although it is different, the average particle diameter is preferably 30 μm or less, and particularly preferably 10 μm or less.
[0031]
Although it does not specifically limit as carbon black used in the manufacturing method of this invention, For example, furnace black, lamp black, thermal black, acetylene black, channel black etc. are mentioned. These may be used alone or in combination of two or more.
[0032]
Next, the thermosetting resin composition of the present invention will be described.
The thermosetting resin composition of the present invention is characterized by containing a thermosetting resin, an inorganic filler, and a carbon black for blending a composition obtained by the production method of the present invention.
[0033]
The thermosetting resin used in the thermosetting resin composition of the present invention (hereinafter sometimes simply referred to as “composition”) is not particularly limited.
Such as phenol novolac resins, cresol novolac resins, bisphenol A novolac resins and other novolac phenol resins, unmodified resole phenol resins, oil-modified resole phenol resins modified with paulownia oil, linseed oil, walnut oil, etc. Phenolic resin,
Orthocresol novolac epoxy resin, phenol novolac epoxy resin, bisphenol epoxy resin, naphthalene epoxy resin, triphenolmethane epoxy resin, triazine nucleus-containing epoxy resin, biphenyl epoxy resin, stilbene epoxy resin, dicyclopentadiene modified Epoxy resins such as phenolic epoxy resins,
Resins having a triazine ring such as urea (urea) resin, melamine resin, unsaturated polyester resin, bismaleimide resin, polyurethane resin, diallyl phthalate resin, silicone resin, resin having a benzoxazine ring, cyanate ester resin,
Etc.
[0034]
Among these, when the thermosetting resin composition is used for sealing an electronic component, an epoxy resin is used. Although it is not specifically limited as an equivalent of the epoxy resin in such a use, It is preferable to use what is 150-300 g / eq from a sclerosing | hardenable viewpoint.
[0035]
Moreover, a hardening | curing agent can be mix | blended with the said thermosetting resin as needed. A well-known hardener can be used according to the kind of each thermosetting resin.
For example, in the case of a novolac type phenol resin, hexamethylenetetramine, paraformaldehyde or the like, and in the case of an epoxy resin, an acid anhydride, a polyamine compound, an imidazole compound, a polyphenol compound such as a phenol resin, or the like can be used.
[0036]
In particular, when the composition is used for sealing an electronic component, a phenol resin is preferably used as a curing agent for the epoxy resin.
Here, the phenol resin is not particularly limited as long as it has a phenolic hydroxyl group in the molecule. For example, phenol novolak resin, phenol aralkyl resin, naphthol aralkyl resin, triphenylmethane resin, dicyclopentadiene-modified phenol resin, Examples include terpene-modified phenolic resins and their modified resins. When these phenol resins are used, those having a hydroxyl equivalent of 80 to 250 g / eq are preferable from the viewpoint of curability.
[0037]
In addition to the above curing agent, a curing accelerator can also be used.
For example, when an epoxy resin is used as the thermosetting resin and a phenol resin is used as the curing agent, the curing accelerator is not particularly limited as long as it accelerates the reaction between the epoxy group and the hydroxyl group. For example, 1,8-diazabicyclo (5,4,0) undecene-7, triphenylphosphine, benzyldimethylamine, 2-methylimidazole, tetraphenylphosphonium tetraphenylborate and the like. These may be used alone or in combination of two or more.
[0038]
The inorganic filler used in the composition of the present invention is not particularly limited. For example, silicates such as talc and calcined clay, oxides such as alumina, silica and fused silica, calcium carbonate, hydrotalcite and the like Carbonates, hydroxides such as aluminum hydroxide and magnesium hydroxide, sulfates such as barium sulfate and calcium sulfite, or borates such as sulfite and zinc borate, and nitrides such as aluminum nitride and silicon nitride Representative inorganic fillers, various thermosetting resins such as phenolic resins, acrylic resins, polyamides, polysulfones, polystyrenes, fluororesins, or powders of thermoplastic resins, or powders such as copolymers composed of these resins Organic typified by fibrous organic fillers such as organic fillers, wood flour, pulp, kenaf, aramid fiber, polyester fiber, etc. Hama material, and the like.
[0039]
Among the fillers, when a composition containing an epoxy resin is used for sealing an electronic component, fused crushed silica, fused spherical silica, crystalline silica, alumina, silicon nitride, or the like can be used. In particular, when the composition is used as a semiconductor encapsulant, fused spherical silica is most preferable from the balance of moldability, reliability to a semiconductor device, thermal expansion coefficient, and the like.
[0040]
The blending amount of each of the above components in the composition of the present invention is not particularly limited, and an optimum range is considered in consideration of the thermosetting resin and curing agent to be used, the type of inorganic filler, or the use of the composition. It can be selected appropriately.
[0041]
In addition to the components listed above, the composition of the present invention includes various additives such as coupling agents, flame retardants, flame retardant aids, mold release agents, and low stress agents other than those used in the production method of the present invention. Can also be used together.
[0042]
The composition of this invention can be manufactured by a normal method. For example, a thermosetting resin, a curing agent, an inorganic filler, carbon black obtained by the production method of the present invention, and other additives are mixed by a mixer and then melt kneaded by a kneading apparatus such as a hot roll or a kneader. It can be obtained by pulverizing after cooling.
[0043]
The composition thus obtained can be applied to sealing, coating, insulation, etc. of various thermosetting resin molded products and electronic parts such as semiconductors.
Although it does not specifically limit as a method to shape | mold using the composition of this invention, Well-known shaping | molding methods, such as injection molding, transfer molding, and compression molding, can be applied.
[0044]
【Example】
Hereinafter, the present invention will be described in detail with reference to examples.
[0045]
1. Production of carbon black for blending compositions
<Example 1>
Carbon black (manufactured by Mitsubishi Chemical Co., Ltd., general-purpose color type), 50 g at a pneumatic pressure of 0.6 MPa using a swirl type impact pulverizer (manufactured by Nippon Pneumatic Industry Co., Ltd., “supersonic jet pulverizer PJM-200SP”) The carbon black particles A were obtained by dispersion treatment at / min.
[0046]
Next, using the apparatus shown in FIG. 2, surface coating treatment with a coupling agent was performed using carbon black particles A and a coupling agent (“TSL-8350” manufactured by Toshiba Silicone Co., Ltd.).
As a spray device for supplying carbon black particles A, “BN-90S1” manufactured by Atmax Co., Ltd. is used, and the air pressure is 4 kg / cm. ² As 100 g / min and a swirling flow was generated in the mixing apparatus. As a nozzle atomizer on the coupling agent supply side, “Magic Cut e-mist (nozzle type FN-Z40)” manufactured by Fuso Seiki Co., Ltd. is used, and the air pressure is 3.0 kg / cm. ² As 23 g / min.
These are mixed by using a cylindrical mixing device having a cylindrical part device inner diameter of 300 mm and a cylindrical part and a truncated cone part each having a height of 250 mm. Carbon black particles B subjected to coating treatment were obtained.
[0047]
In addition, the specification and operation conditions of the apparatus which gives a shear shear force were performed as follows.
(1) Uchiko specifications:
A truncated cone shape having a short diameter side (supply side) outer diameter of 30 mm, a long diameter side (discharge side) outer diameter of 60 mm, and a truncated cone height of 80 mm was used. A groove having a planar shape and a cross-sectional shape shown in FIG. 3 was used. The groove had a cross-sectional width of 5 mm and a depth of 2 mm, and was processed at 12 uniform pitches.
(2) Outer specifications:
It was made into the shape which has the same clearance in all the parts which oppose the inner core which is a truncated cone shape, and the clearance was 0.5 mm. What was not given groove processing was used.
(3) Temperature control conditions for the inner and outer cores: Both the inner and outer cores were set at room temperature.
(4) Operating conditions of the inner core: The rotational speed was 1200 rpm.
[0048]
<Example 2>
The carbon black particles B obtained in Example 1 were mixed with a swirl type impact pulverizer (manufactured by Nippon Pneumatic Kogyo Co., Ltd., “supersonic jet pulverizer PJM-200SP” at an air pressure of 0.6 MPa, 50 g / Dispersion treatment was performed with min to obtain carbon black particles C.
[0049]
<Comparative example>
The carbon black particles used in Example 1 were used as they were without being dispersed.
[0050]
2. Production of the composition
The raw materials shown in Table 1 were mixed at room temperature with a mixer and then melt-kneaded with a heated roll apparatus at 80 to 100 ° C. This was pulverized after cooling to obtain a composition.
[0051]
3. Evaluation
The following items were evaluated for the carbon black and composition obtained above. The results are shown in Table 1.
(1) Average particle diameter of carbon black: Volume average particle diameter was measured using a laser diffraction particle size distribution measuring device “SALD-7000” manufactured by Shimadzu Corporation.
(2) Spiral flow of composition: Using a mold conforming to EMMI-I-66, it was measured by molding under conditions of a mold temperature of 175 ° C., an injection pressure of 7 MPa, and a pressure holding time of 120 seconds.
(3) Measurement of carbon black particle diameter in the molded composition: using a low-pressure transfer molding apparatus, a disk with a mold temperature of 175 ° C., an injection pressure of 6.9 MPa, a holding time of 120 seconds, 100 mmφ, and a thickness of 3 mm Was molded. The disk surface was surface polished using a diamond pad. The polished surface was observed using a fluorescence microscope (OLYMPUS, “BX51M-53MF”), and the number of carbon blacks having a particle diameter within a predetermined range was measured. This was performed on two disks and the average value was calculated.
[0052]
[Table 1]

[0053]
<Notes on the table>
(1) Epoxy resin: “YX4000H” manufactured by Japan Epoxy Resin Co., Ltd. (biphenyl type epoxy resin, melting point 105 ° C., epoxy equivalent 195 g / eq)
(2) Curing agent: novolac type phenol resin (softening point 65 ° C., hydroxyl group equivalent 104)
[0054]
Examples 1 and 2 are carbon blacks obtained by the production method of the present invention in which carbon black is dispersed with an impact pulverizer and then the surface thereof is coated with a coupling agent. Compared to the comparative example used, the average particle size was small and the dispersibility was excellent.
[0055]
【The invention's effect】
The present invention is a method for producing a carbon black for blending a composition characterized in that carbon black is dispersed with an impact pulverizer and then the surface thereof is coated with a coupling agent. Can be effectively dispersed and re-aggregation can be suppressed. The carbon black obtained by the method for producing a carbon black for blending a composition of the present invention is particularly preferably used for, for example, a thermosetting resin composition material for encapsulating electronic components that require high insulation performance. It can be done.
[Brief description of the drawings]
FIG. 1 (a) Carbon black supply device (side sectional view)
(B) Coupling agent supply device (side sectional view)
FIG. 2 shows an example of an apparatus for coating the surface of carbon black with a coupling agent (side sectional view).
FIG. 3 (a) Groove shape of inner surface of device for applying shear shear force (side view)
(B) Groove shape (cross-sectional view) of the inner surface of the device for applying a shear shear force
[Explanation of symbols]
1 carbon black
5 Spray equipment
11 Coupling agent
13 Nozzle atomizer
21 Mixing equipment
31 Device for applying shearing shear force

Claims (4)

A method for producing carbon black for blending a composition, characterized in that carbon black is subjected to a dispersion treatment with an impact pulverizer and then the surface is coated with a coupling agent. A method for producing carbon black for blending a composition, characterized in that after carbon black is dispersed with an impact pulverizer, the surface thereof is coated with a coupling agent, and further dispersed with an impact pulverizer. . The method for producing a carbon black for blending a composition according to claim 1 or 2, wherein the impact pulverizer is a jet mill. A thermosetting resin composition comprising a thermosetting resin, an inorganic filler, and carbon black for blending a composition obtained by the production method according to claim 1.

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