JP2000191317A - Production of fused spherical silica - Google Patents
Production of fused spherical silicaInfo
- Publication number
- JP2000191317A JP2000191317A JP36834198A JP36834198A JP2000191317A JP 2000191317 A JP2000191317 A JP 2000191317A JP 36834198 A JP36834198 A JP 36834198A JP 36834198 A JP36834198 A JP 36834198A JP 2000191317 A JP2000191317 A JP 2000191317A
- Authority
- JP
- Japan
- Prior art keywords
- silica
- crushed
- fumed silica
- spherical silica
- fused spherical
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- Silicon Compounds (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、溶融球状シリカの
製造方法に関する。さらに詳しくは、諸性質の制御が容
易で、生産性が大幅に向上した溶融球状シリカを破砕シ
リカから製造する方法に関する。[0001] The present invention relates to a method for producing fused spherical silica. More particularly, the present invention relates to a method for producing fused spherical silica from crushed silica in which various properties are easily controlled and productivity is greatly improved.
【０００２】[0002]
【従来の技術】従来より、半導体封止用樹脂組成物のフ
ィラーとして、シリカを主体とするフィラーが使用され
ている。そして、半導体の高集積度化に伴って、上記し
たフィラーをより高充填した半導体封止用樹脂組成物が
求められている。2. Description of the Related Art Conventionally, a filler mainly composed of silica has been used as a filler of a resin composition for encapsulating a semiconductor. With the increase in the degree of integration of semiconductors, there is a demand for a resin composition for semiconductor encapsulation in which the above-mentioned filler is further filled.
【０００３】そして近年、高充填化するためのフィラー
として、球状シリカを主体とするフィラーが研究・開発
されている。上記した球状シリカを製造する方法のひと
つとして、破砕シリカを溶融させて球状化させる方法が
行われている。In recent years, fillers mainly composed of spherical silica have been studied and developed as fillers for high filling. As one of the methods for producing the above-mentioned spherical silica, a method of melting crushed silica to make it spherical.
【０００４】通常、破砕シリカを溶融させて球状シリカ
を製造する方法として、特開平２−１４５５１５号公報
や特開平８−１１９６１８号公報に記載されているよう
に、破砕シリカを、酸素−可燃性ガスによる火炎に供給
して溶融する方法が採用される。しかしながら、破砕シ
リカを火炎により溶融する際、破砕シリカの流動性不足
のため、破砕シリカの供給速度が不安定になるという問
題が発生する。そのため、上記方法では、得られる球状
シリカの性質を制御するのが困難であったり、製造が定
常的に行えないという問題があった。[0004] Usually, as a method for producing spherical silica by melting crushed silica, as described in JP-A-2-145515 and JP-A-8-119618, crushed silica is treated with oxygen-flammable silica. A method of supplying a gas flame and melting it is adopted. However, when the crushed silica is melted by a flame, there is a problem that the supply speed of the crushed silica becomes unstable due to insufficient fluidity of the crushed silica. Therefore, in the above-mentioned method, there were problems that it was difficult to control the properties of the obtained spherical silica and that the production could not be performed constantly.
【０００５】[0005]
【発明が解決しようとする課題】したがって、破砕シリ
カから球状シリカを製造する方法において、生産性がよ
い製造方法、すなわち、製造が定常的に行え、得られる
球状シリカの性質を制御できる製造方法が求められてき
た。Therefore, in the method of producing spherical silica from crushed silica, a production method with good productivity, that is, a production method in which production can be performed constantly and the properties of the obtained spherical silica can be controlled. I have been asked.
【０００６】[0006]
【課題を解決するための手段】本発明者等は、上記課題
に鑑み、鋭意研究した結果、破砕シリカに煙霧シリカを
混合した原料を用いることにより、上記課題が解決でき
ることを見出し、本発明を完成するに至った。Means for Solving the Problems The present inventors have conducted intensive studies in view of the above problems, and as a result, have found that the above problems can be solved by using a raw material obtained by mixing fumed silica with crushed silica. It was completed.
【０００７】すなわち、本発明は、破砕シリカに煙霧シ
リカを添加し、混合した後、火炎中に供給することを特
徴とする溶融球状シリカの製造方法である。That is, the present invention is a method for producing fused spherical silica, wherein fumed silica is added to crushed silica, mixed, and then supplied into a flame.
【０００８】本発明で用いられる破砕シリカは、特に限
定されず、合成シリカおよび／または天然シリカを原料
とするものが好適に用いられる。上記合成シリカとして
は、ハロゲン化シランの加水分解によるもの、オルガノ
シリケートの加水分解によるもの、珪酸アルカリの中和
によるものが挙げられ、上記天然シリカとしては、珪
石、珪砂、水晶等が挙げられる。また、上記破砕シリカ
は、通常、これら原料を、ジェットミルやボールミル等
の公知の方法で破砕したものとして使用できる。[0008] The crushed silica used in the present invention is not particularly limited, and those using synthetic silica and / or natural silica as a raw material are suitably used. Examples of the synthetic silica include those obtained by hydrolysis of a halogenated silane, those obtained by hydrolysis of an organosilicate, and those obtained by neutralization of an alkali silicate. Examples of the natural silica include silica stone, silica sand, and quartz. In addition, the above-mentioned crushed silica can be usually used as those obtained by crushing these raw materials by a known method such as a jet mill or a ball mill.
【０００９】上記破砕シリカの平均粒径は、特に限定さ
れず、必要とする球状シリカの平均粒径を勘案して適宜
決定すればよい。通常、平均粒径２〜６０μｍのものが
好適であり、より好ましくは３〜２０μｍである。な
お、通常、火炎溶融方法により得られる球状シリカの平
均粒径や粒度分布は、原料として使用される破砕シリカ
の平均粒径や粒度分布とほぼ等しくなる。The average particle size of the crushed silica is not particularly limited, and may be appropriately determined in consideration of the required average particle size of the spherical silica. Usually, those having an average particle size of 2 to 60 μm are suitable, and more preferably 3 to 20 μm. In addition, usually, the average particle diameter and particle size distribution of the spherical silica obtained by the flame melting method are almost equal to the average particle diameter and particle size distribution of the crushed silica used as a raw material.
【００１０】一方、本発明で用いられる煙霧シリカは、
いわゆるシラン化合物を気相加水分解して得られるシリ
カである。上記煙霧シリカの原料であるシラン化合物と
しては、公知のものが特に制限なく使用できる。例え
ば、テトラクロロシラン、トリクロロシラン、ジクロロ
シランの如きハロゲン化シランあるいはモノメチルトリ
クロロシランなどの揮発性を有しかつ加水分解可能なシ
ラン化合物であればいずれでもよい。On the other hand, the fumed silica used in the present invention is:
This is silica obtained by so-called gas phase hydrolysis of a silane compound. As the silane compound which is a raw material of the fumed silica, known compounds can be used without any particular limitation. For example, any volatile and hydrolyzable silane compounds such as halogenated silanes such as tetrachlorosilane, trichlorosilane and dichlorosilane or monomethyltrichlorosilane may be used.
【００１１】上記煙霧シリカの比表面積は、特に限定さ
れないが、生産性等を勘案すると、１００ｍ2／ｇ以上
のものが好適に用いられる。また、上記煙霧シリカは、
生産性等を勘案すると、表面が疎水化処理されているこ
とが好ましい。上記疎水化処理は、一般的に疎水化剤と
して用いられている有機珪素化合物、例えばヘキサメチ
ルジシラザン、テトラシクロシロキサン、トリメチルク
ロロシラン、ジメチルジクロロシラン等により行われ
る。疎水化処理としては、それ自体公知の方法が採用さ
れる。The specific surface area of the fumed silica is not particularly limited, but preferably 100 m 2 / g or more in consideration of productivity and the like. Also, the fume silica is
In consideration of productivity and the like, the surface is preferably subjected to a hydrophobic treatment. The hydrophobization treatment is performed using an organic silicon compound generally used as a hydrophobizing agent, for example, hexamethyldisilazane, tetracyclosiloxane, trimethylchlorosilane, dimethyldichlorosilane, or the like. As the hydrophobizing treatment, a method known per se is employed.
【００１２】本発明において、上記破砕シリカと煙霧シ
リカとを混合することにより、生産性のよい溶融球状シ
リカを製造することができる。本発明において、破砕シ
リカと煙霧シリカの混合割合は、特に限定されないが、
破砕シリカと煙霧シリカの合計重量を基準にして、破砕
シリカが９９.５〜７０重量％でありそして煙霧シリカ
が０.５〜３０重量％の範囲であることが好適である。In the present invention, by mixing the above-mentioned crushed silica and fumed silica, fused spherical silica having good productivity can be produced. In the present invention, the mixing ratio of crushed silica and fumed silica is not particularly limited,
It is preferred that the crushed silica is in the range of 99.5 to 70% by weight and the fumed silica is in the range of 0.5 to 30% by weight, based on the combined weight of crushed silica and fumed silica.
【００１３】煙霧シリカの配合量が０.５重量％未満の
場合、生産性が向上し難いため好ましくなく、配合量が
３０重量％を越えると、得られる溶融球状シリカの流動
分布等の諸性質が変化し易くなるので好ましくない。ま
た上記破砕シリカと煙霧シリカの混合方法は、特に限定
されず、それ自体公知の方法が用いられる。When the amount of the fumed silica is less than 0.5% by weight, it is not preferable because the productivity is hardly improved. When the amount of the fumed silica exceeds 30% by weight, various properties such as flow distribution of the obtained fused spherical silica are obtained. Is not preferred because it tends to change. The method for mixing the crushed silica and the fumed silica is not particularly limited, and a method known per se is used.
【００１４】本発明において、上記した破砕シリカと煙
霧シリカとの混合物を、火炎中に供給し溶融する方法と
しては、それ自体公知の方法が用いられる。例えば、特
公平３−３６７６１号公報に記載されている方法、すな
わち気体または液体燃料に、酸素または空気などの支燃
ガスを混合しそしてバーナーにて燃焼させた火炎中に、
エジェクター、スクリューフィーダー、流動層を用いる
方法により原料シリカを供給して溶融させ、溶融球状シ
リカを生成させ、該溶融球状シリカをサイクロンに導い
て固気分離する方法が好適である。In the present invention, as a method of supplying the above-mentioned mixture of crushed silica and fumed silica into a flame and melting the same, a method known per se is used. For example, a method described in Japanese Patent Publication No. 3-37661, that is, a gas or liquid fuel mixed with a supporting gas such as oxygen or air and burned with a burner,
It is preferable to use a method using an ejector, a screw feeder, and a fluidized bed to supply and melt raw material silica to generate fused spherical silica, and to guide the fused spherical silica to a cyclone to perform solid-gas separation.
【００１５】[0015]
【実施例】本発明を具体的に説明するために実施例を示
すが、本発明はこれらの実施例に限定されるものではな
い。なお、実施例および比較例中での評価は、以下のよ
うに行った。EXAMPLES The present invention will be described in more detail with reference to Examples, but it should be understood that the present invention is by no means restricted to such specific Examples. In addition, the evaluation in an Example and a comparative example was performed as follows.
【００１６】・平均粒径 ＳＫ ＬＡＳＥＲ ＰＲＯ−７０００（セイシン企業
製）を用い、レーザー回折散乱法により測定した。 ・粒子形状 ＳＥＭにより測定した。 ・供給状況 供給機の内部圧力の変動と、火炎の濃淡の変動により評
価した。Average particle diameter Measured by a laser diffraction scattering method using SK LASER PRO-7000 (manufactured by Seishin Enterprise). -Particle shape It measured by SEM.・ Supply situation The evaluation was made based on the fluctuation of the internal pressure of the feeder and the fluctuation of the concentration of the flame.
【００１７】実施例１ 以下のような操作を行い溶融球状シリカを得た。まず、
平均粒径８μｍの球状シリカをボールミルで粉砕した破
砕シリカ（平均粒径５.７μｍ、比表面積３.０ｍ2／
ｇ）９９重量％と、煙霧シリカ（比表面積２００ｍ2／
ｇ）１重量％を混合し、原料シリカを得た。Example 1 The following operations were performed to obtain fused spherical silica. First,
A crushed silica obtained by pulverizing a spherical silica having an average particle size of 8 μm with a ball mill (average particle size of 5.7 μm, specific surface area of 3.0 m 2 /
g) 99% by weight and fumed silica (specific surface area: 200 m 2 /
g) 1% by weight was mixed to obtain a raw material silica.
【００１８】次いで、中心管、円周管、外周管からなる
３重管バーナーを設置した円筒状溶融炉を用い、得られ
た原料シリカ（供給速度１.０ｋｇ／ｈ）を酸素（流量
４ｍ3／ｈ）と共に同伴させて円周管より導入し、水素
３（流速８ｍ3／ｈ）を中心管および外周管より供給し
て、火炎を形成させて溶融し、粗溶融シリカを得た。そ
して、得られた租溶融シリカをサイクロンに導入し、固
気分離を行い溶融球状シリカを得た。結果を表１に示
す。なお、得られた溶融球状シリカの粒度分布は、破砕
シリカの粒度分布とほぼ同じであった。Then, using a cylindrical melting furnace equipped with a triple tube burner consisting of a center tube, a circumferential tube and an outer tube, the obtained raw material silica (feed rate: 1.0 kg / h) was converted to oxygen (flow rate: 4 m 3). / H) and hydrogen gas (flow rate: 8 m 3 / h) was supplied from the central pipe and the outer peripheral pipe to form a flame and melt to obtain coarse fused silica. The obtained fused silica was introduced into a cyclone, and subjected to solid-gas separation to obtain fused spherical silica. Table 1 shows the results. The particle size distribution of the obtained fused spherical silica was almost the same as the particle size distribution of the crushed silica.
【００１９】実施例２ 原料シリカの供給量を２.０ｋｇ／ｈとした以外は、実
施例１と同様の操作を行った。結果を表１に示す。Example 2 The same operation as in Example 1 was performed except that the supply amount of the raw material silica was 2.0 kg / h. Table 1 shows the results.
【００２０】実施例３ 煙霧シリカの量を５重量％、原料シリカの供給量を２.
１ｋｇ／ｈとした以外は、実施例１と同様の操作を行っ
た。結果を表１に示す。Example 3 The amount of fumed silica was 5% by weight and the amount of raw material silica was 2.
Except for 1 kg / h, the same operation as in Example 1 was performed. Table 1 shows the results.
【００２１】実施例４ 煙霧シリカの量を４０重量％とした以外は、実施例１と
同様の操作を行った。結果を表１に示す。なお、得られ
た溶融球状シリカの粒度分布は、破砕シリカの粒度分布
とは異なっていた。Example 4 The same operation as in Example 1 was performed except that the amount of fumed silica was changed to 40% by weight. Table 1 shows the results. In addition, the particle size distribution of the obtained fused spherical silica was different from the particle size distribution of the crushed silica.
【００２２】実施例５ ヘキサメチルジシラザンで処理した疎水化煙霧シリカを
用いた以外は、実施例１と同様の操作を行った結果を表
１に示す。Example 5 The results obtained by performing the same operation as in Example 1 except that hydrophobized fumed silica treated with hexamethyldisilazane was used are shown in Table 1.
【００２３】比較例１ 煙霧シリカを添加しない以外は、実施例１と同様の操作
を行った。結果を表１に示す。結果として、安定的に生
産できず、また粒子同士がくっついた塊状粒子がみられ
た。Comparative Example 1 The same operation as in Example 1 was performed except that no fumed silica was added. Table 1 shows the results. As a result, stable production was not possible, and massive particles in which the particles stuck together were observed.
【００２４】[0024]
【表１】 [Table 1]
【００２５】表１に示すとおり、煙霧シリカを配合した
破砕シリカを用いると、安定的に製造でき、また得られ
る溶融シリカも、ほぼ真球状であった。一方、煙霧シリ
カを配合していない破砕シリカでは、安定的に生産でき
ず、さらに得られる溶融シリカも塊状粒子がみられた。As shown in Table 1, when crushed silica containing fumed silica was used, stable production was possible, and the obtained fused silica was almost spherical. On the other hand, the crushed silica containing no fumed silica could not be produced stably, and the resulting fused silica was also found to have massive particles.
【００２６】[0026]
【発明の効果】本発明の方法によれば、生産性良く溶融
シリカを製造することができる。さらに、本発明の方法
により得られる溶融シリカは、塊状物が非常に少ないの
で、エポキシ樹脂等に配合した場合、樹脂を流動性の良
好なものにできる。According to the method of the present invention, fused silica can be produced with high productivity. Further, since the fused silica obtained by the method of the present invention has very few lumps, when blended with an epoxy resin or the like, the resin can have good fluidity.
フロントページの続き (72)発明者 青木 博男 山口県徳山市御影町１番１号 株式会社ト クヤマ内 (72)発明者 三上 直樹 山口県徳山市御影町１番１号 株式会社ト クヤマ内 Ｆターム(参考） 4G072 AA25 AA28 BB07 CC16 DD03 DD04 GG03 HH14 LL05 MM02 MM38 QQ07 RR11 TT01 TT05 UU09 Continued on the front page (72) Inventor Hiroo Aoki 1-1, Mikage-cho, Tokuyama-shi, Yamaguchi Prefecture Inside Tokuyama Corporation (72) Inventor Naoki Mikami 1-1, Mikage-cho, Tokuyama-shi, Yamaguchi Prefecture Tokuyama Corporation F term (reference) 4G072 AA25 AA28 BB07 CC16 DD03 DD04 GG03 HH14 LL05 MM02 MM38 QQ07 RR11 TT01 TT05 UU09
Claims (5)
した後、火炎中に供給することを特徴とする溶融球状シ
リカの製造方法。1. A method for producing fused spherical silica, comprising adding fumed silica to crushed silica, mixing the fumed silica, and supplying the mixed fumed silica into a flame.
範囲である請求項１記載の溶融球状シリカの製造方法。2. The method for producing fused spherical silica according to claim 1, wherein the average particle size of the crushed silica is in the range of 2 to 60 μm.
以上である請求項１記載の溶融球状シリカの製造方法。3. The specific surface area of the fumed silica is 100 m 2 / g.
The method for producing fused spherical silica according to claim 1, which is as described above.
霧シリカの合計量に基づいて、０.５〜３０重量％の範
囲である請求項１記載の溶融球状シリカの製造方法。4. The method according to claim 1, wherein the amount of the fumed silica is in the range of 0.5 to 30% by weight based on the total amount of the crushed silica and the fumed silica.
性煙霧シリカである請求項１記載の溶融球状シリカの製
造方法。5. The method for producing fused spherical silica according to claim 1, wherein the fumed silica is hydrophobic fumed silica whose surface is hydrophobized.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP36834198A JP4030668B2 (en) | 1998-12-25 | 1998-12-25 | Method for producing fused spherical silica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP36834198A JP4030668B2 (en) | 1998-12-25 | 1998-12-25 | Method for producing fused spherical silica |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2000191317A true JP2000191317A (en) | 2000-07-11 |
| JP4030668B2 JP4030668B2 (en) | 2008-01-09 |
Family
ID=18491576
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP36834198A Expired - Fee Related JP4030668B2 (en) | 1998-12-25 | 1998-12-25 | Method for producing fused spherical silica |
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| Country | Link |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007015884A (en) * | 2005-07-07 | 2007-01-25 | Micron:Kk | Method and apparatus for manufacturing spherical fine inorganic powder |
| JP2009137798A (en) * | 2007-12-06 | 2009-06-25 | Admatechs Co Ltd | Method and apparatus for manufacturing spherical inorganic substance powder and method for preparing resin composition |
| JP2009227504A (en) * | 2008-03-21 | 2009-10-08 | Admatechs Co Ltd | Spherical low-melting point glass composition powder, manufacturing method, and low-melting point glass composition |
| ITBO20100169A1 (en) * | 2010-03-17 | 2011-09-18 | Teuco Guzzini Spa | PROCEDURE FOR THE REALIZATION OF COMPOSITE MATERIAL AND COMPOSITE MATERIAL THAT CAN BE OBTAINED |
| JP2013035751A (en) * | 2012-10-01 | 2013-02-21 | Admatechs Co Ltd | Method and apparatus for producing spherical inorganic material powder, and method for producing resin composition |
| JP2015086120A (en) * | 2013-10-31 | 2015-05-07 | 株式会社トクヤマ | Spherical silica fine powder and production method thereof |
-
1998
- 1998-12-25 JP JP36834198A patent/JP4030668B2/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007015884A (en) * | 2005-07-07 | 2007-01-25 | Micron:Kk | Method and apparatus for manufacturing spherical fine inorganic powder |
| JP2009137798A (en) * | 2007-12-06 | 2009-06-25 | Admatechs Co Ltd | Method and apparatus for manufacturing spherical inorganic substance powder and method for preparing resin composition |
| JP2009227504A (en) * | 2008-03-21 | 2009-10-08 | Admatechs Co Ltd | Spherical low-melting point glass composition powder, manufacturing method, and low-melting point glass composition |
| ITBO20100169A1 (en) * | 2010-03-17 | 2011-09-18 | Teuco Guzzini Spa | PROCEDURE FOR THE REALIZATION OF COMPOSITE MATERIAL AND COMPOSITE MATERIAL THAT CAN BE OBTAINED |
| EP2366731A1 (en) * | 2010-03-17 | 2011-09-21 | DELTA s.r.l. | A process for preparing a composite material and composite material obtained |
| JP2013035751A (en) * | 2012-10-01 | 2013-02-21 | Admatechs Co Ltd | Method and apparatus for producing spherical inorganic material powder, and method for producing resin composition |
| JP2015086120A (en) * | 2013-10-31 | 2015-05-07 | 株式会社トクヤマ | Spherical silica fine powder and production method thereof |
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