JPH01234320A - Production of spherical silica - Google Patents
Production of spherical silicaInfo
- Publication number
- JPH01234320A JPH01234320A JP6058188A JP6058188A JPH01234320A JP H01234320 A JPH01234320 A JP H01234320A JP 6058188 A JP6058188 A JP 6058188A JP 6058188 A JP6058188 A JP 6058188A JP H01234320 A JPH01234320 A JP H01234320A
- Authority
- JP
- Japan
- Prior art keywords
- particles
- resin
- silica
- spherical silica
- coarse particles
- 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.)
- Pending
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
- 239000002245 particle Substances 0.000 claims abstract description 16
- 239000002184 metal Substances 0.000 claims abstract description 6
- 229910052751 metal Inorganic materials 0.000 claims abstract description 6
- 230000004927 fusion Effects 0.000 claims description 8
- 239000011362 coarse particle Substances 0.000 abstract description 15
- 239000012798 spherical particle Substances 0.000 abstract description 4
- 239000004115 Sodium Silicate Substances 0.000 abstract description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052911 sodium silicate Inorganic materials 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 10
- 239000011164 primary particle Substances 0.000 description 8
- 238000007751 thermal spraying Methods 0.000 description 4
- 239000004677 Nylon Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 239000011163 secondary particle Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 239000005062 Polybutadiene Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
- C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
- Silicon Polymers (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明は樹脂充填材等として有用な球状シリカの製造方
法に関するものである。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for producing spherical silica useful as a resin filler and the like.
従来の技術
球状シリカはＩＣ封止材、磁気テープ等の各種樹脂の充
填材や液晶パネルのギャップ材等として多くの分野で利
用されている。そして、このような球状シリカについて
は一次粒子間の凝集あるいは部分的な融着により生じた
粗大粒子を含まないこと、および比表面積が小′さいこ
と等の条件が要求されることが多い。BACKGROUND OF THE INVENTION Spherical silica is used in many fields as an IC sealant, a filler for various resins such as magnetic tape, and a gap material for liquid crystal panels. Such spherical silica is often required to be free from coarse particles resulting from aggregation or partial fusion between primary particles, and to have a small specific surface area.
非孔性球状シリカを製造する方法としては、例えばハロ
ゲノシラン化合物を水蒸気分解する方法、スプレードラ
イ法、破砕シリカの溶射法等が知られているが、これら
の方法に使用されるドライゲルはいずれも比表面積が１
００ｒｒｒ／ｇ以上と大きいため、８００℃以上の高温
で焼成および／又は１７００℃以上の高温で溶射処理を
行い、粒子の内部又は表面を焼結して比表面積を１０ｎ
？／ｇ以下、好ましくは３ｒｄ／ｇ以下とする必要があ
る。Known methods for producing non-porous spherical silica include, for example, a method of steam decomposition of a halogenosilane compound, a spray drying method, a thermal spraying method of crushed silica, etc. However, the dry gel used in these methods is Specific surface area is 1
Since the particles are large at over 00rrr/g, they are fired at a high temperature of 800°C or higher and/or thermal sprayed at a high temperature of 1700°C or higher to sinter the inside or surface of the particles to reduce the specific surface area to 10n.
? /g or less, preferably 3rd/g or less.
焼成又は溶射処理はさまざまな方法が検討され、実施さ
れているが、いずれの方法においても高温処理したのち
に、粒子の内部又は表面の焼結と共に、粒子界面におい
ても部分的に焼結が進行し、融着を生じ、目的とする球
状シリカとは粒径も形状も異なった粗大粒子が混じるこ
ととなる。この粗大粒子の存在は樹脂充填材として用い
た場合、本来球状シリカが持つべき高充填性、コンパウ
ンドの高流動性等という優れた特徴を失わせる。Various methods have been studied and implemented for firing or thermal spraying, but in all methods, after high-temperature treatment, sintering progresses not only inside or on the surface of the particles but also partially at the particle interfaces. However, fusion occurs, and coarse particles having a different particle size and shape from the target spherical silica are mixed. When used as a resin filler, the presence of these coarse particles causes the spherical silica to lose its excellent characteristics such as high filling properties and high fluidity of the compound.
発明が解決しようとする課題
本発明は焼成又は溶射処理されたシリカに含まれる粗大
粒子を解砕して、粗大粒子を含まない球状シリカの製造
方法を提供することを目的とする。Problems to be Solved by the Invention An object of the present invention is to provide a method for producing spherical silica free of coarse particles by crushing coarse particles contained in fired or thermally sprayed silica.
−課題を解決するための手段
本発明は、珪素質微小球状粒子を８００℃以上の高温で
焼成および／又は１７００℃以上の高温で溶射処理する
とき生成する粒子間の部分的な融着により生じた粗大シ
リカ粒子を、樹脂ボールおよび／又は樹脂コートした金
属芯ボールを用いる粉砕機を使用して前記部分的な融着
により生じた粗大シリカ粒子を選択的に解砕することに
より粗大シリカ粒子を含まない球状シリカを製造方法で
ある。- Means for Solving the Problems The present invention provides a solution to the problems caused by partial fusion between particles generated when silicon microspherical particles are fired at a high temperature of 800°C or higher and/or thermal sprayed at a high temperature of 1700°C or higher. The coarse silica particles produced by the partial fusion are selectively crushed using a crusher using resin balls and/or resin-coated metal core balls. This is a method for producing spherical silica that does not contain spherical silica.
珪素質微小球状粒子は珪酸ナトリウム、テトラアルコキ
シシラン、ハロゲノシラン化合物等の原料から公知の方
法によって製造したものや、天然シリカを破砕したもの
など任意のものが使用でき焼成はシリカの焼結が起こる
８００℃以上の高温で行も、また、溶射処理は通常の温
度である１７００℃以上で行う、いずれも、公知の条件
で差支えない。The siliceous microspherical particles can be made from materials such as sodium silicate, tetraalkoxysilane, or halogenosilane compounds by known methods, or crushed natural silica, or any other material can be used.Sintering of the silica occurs during firing. The thermal spray treatment may be carried out at a high temperature of 800° C. or higher, or the thermal spraying may be carried out at a normal temperature of 1700° C. or higher, both of which may be carried out under known conditions.
焼成又は溶射処理により、シリカ粒子（１次粒子）が部
分的に融着して粗大粒子（２次粒子）が生ずる０本発明
はこの１次粒子はできるだけ粉砕することなく、２次粒
子のできるだけ全部を１次粒子にまで解砕するものであ
る。その目的のため樹脂ボールおよび／又は樹脂コート
した金属芯ボールを用いる粉砕機を使用して解砕する。By baking or thermal spraying, silica particles (primary particles) are partially fused to form coarse particles (secondary particles).The present invention aims to reduce the amount of secondary particles as much as possible without pulverizing these primary particles. This is to crush everything into primary particles. For that purpose, it is crushed using a crusher using resin balls and/or resin-coated metal core balls.
このような融着による粗大粒子を解砕する手段として、
超音波振動による方法、ボールミルを使用する方法など
が考えられるが、前者は解砕力が十分でなく、また湿式
であるために後処理が必要であり、後者は衝撃力が強力
であって１次粒子までを粉砕してしまう、 本発明で使
用する樹脂ボールおよび／又は樹脂コートした金属芯ボ
ールを用いる粉砕機はその衝撃力が適当であって、１次
粒子の破砕はもたらさず、２次粒子のみを解砕するこた
ができる。この場合、ボールの大きさは１ｍｍから数ｃ
ｍまでのものが使用できる。粉砕機としては、ボールミ
ル、振動ミルなどが挙げられる。また、ボールミルとし
ては、回転式のもの、振動式のものいずれも用いること
ができる。ボールに使用される樹脂としては、ナイロン
、ポリエステル、ポリブタジェンなど耐衝撃性に優れる
ものが好ましい。As a means of crushing coarse particles caused by such fusion,
Possible methods include using ultrasonic vibration and using a ball mill, but the former does not have sufficient crushing force and requires post-processing because it is a wet method, while the latter has a strong impact force that destroys primary particles. The crusher using resin balls and/or resin-coated metal core balls used in the present invention has an appropriate impact force, and does not crush primary particles, but only secondary particles. It can be used to disintegrate. In this case, the size of the ball is from 1 mm to several centimeters.
Can be used up to m. Examples of the crusher include a ball mill, a vibration mill, and the like. Further, as the ball mill, either a rotary type or a vibrating type can be used. The resin used for the ball is preferably one with excellent impact resistance, such as nylon, polyester, or polybutadiene.
実施例
実施例１
０．２μｍの単分散球状シリカを含むシリカゾルをスプ
レードライヤーで造粒乾燥して、平粒径２０μｍの球状
粒子を得、これを、１２５０℃で１時間焼成した。Examples Example 1 A silica sol containing monodispersed spherical silica of 0.2 μm was granulated and dried with a spray dryer to obtain spherical particles with an average particle diameter of 20 μm, which were then calcined at 1250° C. for 1 hour.
焼成処理したシリカを顕微鏡で観察したところ、粗大粒
子が多く存在し、篩分したところ２００メフシエオーバ
ーのものが５Ｑｗｔ％以上存在した。When the calcined silica was observed under a microscope, it was found that many coarse particles were present, and when it was sieved, it was found that 5 Qwt% or more of silica with a particle size of 200 mesh or more was present.
この２００メツシユオーバーの粗大粒子３００ｇと直径
１０ｍｍのナイロンボール５００ｇをボールミルに入れ
て１１００ｒｐで１時間解砕処理した。これを、再び分
級したところ２００メツシユオーバーのものは５ｗｔ％
であった。また、２００メツシユアンダーのものを顕微
鏡で観察したところ、球状を保ったままであり、１次粒
子が破砕されているものは殆ど見当たらなかった。300 g of these 200 mesh over coarse particles and 500 g of nylon balls with a diameter of 10 mm were placed in a ball mill and crushed at 1100 rpm for 1 hour. When this was classified again, those with 200 mesh over were 5wt%.
Met. Furthermore, when the particles under 200 mesh were observed under a microscope, they remained spherical, and there were hardly any crushed primary particles.
実施例２
実施例１と同じ２００メツシユオーバーの粗大粒子３０
０ｇと直径１５ｍｍのナイロン樹脂コートした鉄芯ボー
ルＩｋｇを振動ボールミルに入れて、振幅５ｍｍ、振動
数１２０Ｏｒｐｍで１時間解砕処理した。これを、再び
分級したところ２００メツシユオーバーのものは４ｗｔ
％であった。Example 2 Same as Example 1, 200 mesh over coarse particles 30
I kg of iron core balls coated with nylon resin and having a diameter of 0 g and a diameter of 15 mm were placed in a vibrating ball mill and crushed at an amplitude of 5 mm and a vibration frequency of 120 rpm for 1 hour. When I classified this again, the one with 200 mesh over was 4wt.
%Met.
また、２００メツシユアンダーのものを顕微鏡で観察し
たところ、球状を保ったままであり、１次粒子が破砕さ
れているものは殆ど見当たらなかった。Furthermore, when the particles under 200 mesh were observed under a microscope, they remained spherical, and there were hardly any crushed primary particles.
（発明の効果〕
本発明によれば、融着による粗大粒子をほとんど含まな
い珪＃Ｉ質微小球状粒子を高歩留で容易に製造すること
ができる。(Effects of the Invention) According to the present invention, silicon #I fine spherical particles containing almost no coarse particles due to fusion can be easily produced at a high yield.
特許出願人 新日鐵化学株式会社Patent applicant Nippon Steel Chemical Co., Ltd.
Claims (1)
よび／又は１７００℃以上の高温で溶射処理するとき生
成する粒子間の部分的な融着により生じた粗大シリカ粒
子を、樹脂ボールおよび／又は樹脂コートした金属芯ボ
ールを用いる粉砕機を使用して前記部分的な融着により
生じた粗大シリカ粒子を選択的に解砕することを特徴と
する球状シリカの製造方法。1. Coarse silica particles produced by partial fusion between particles produced when siliceous microspherical particles are fired at a high temperature of 800°C or higher and/or thermal sprayed at a high temperature of 1700°C or higher are removed by resin balls and/or Alternatively, a method for producing spherical silica, comprising selectively crushing coarse silica particles produced by the partial fusion using a crusher using resin-coated metal core balls.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6058188A JPH01234320A (en) | 1988-03-16 | 1988-03-16 | Production of spherical silica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6058188A JPH01234320A (en) | 1988-03-16 | 1988-03-16 | Production of spherical silica |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01234320A true JPH01234320A (en) | 1989-09-19 |
Family
ID=13146350
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6058188A Pending JPH01234320A (en) | 1988-03-16 | 1988-03-16 | Production of spherical silica |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01234320A (en) |
-
1988
- 1988-03-16 JP JP6058188A patent/JPH01234320A/en active Pending
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