JP2014088298A - Method of producing silica slurry - Google Patents
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- JP2014088298A JP2014088298A JP2012240482A JP2012240482A JP2014088298A JP 2014088298 A JP2014088298 A JP 2014088298A JP 2012240482 A JP2012240482 A JP 2012240482A JP 2012240482 A JP2012240482 A JP 2012240482A JP 2014088298 A JP2014088298 A JP 2014088298A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 238000000034 method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 83
- 239000010453 quartz Substances 0.000 claims abstract description 80
- 239000002002 slurry Substances 0.000 claims abstract description 46
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims description 24
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 238000004898 kneading Methods 0.000 abstract description 24
- 238000003756 stirring Methods 0.000 abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 239000002245 particle Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000012530 fluid Substances 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- METIGIXCFPEQNM-UHFFFAOYSA-M amino-(2-bromoethyl)-dimethylazanium;bromide Chemical compound [Br-].C[N+](C)(N)CCBr METIGIXCFPEQNM-UHFFFAOYSA-M 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
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Abstract
Description
本発明は、凝集体の少ない均一なシリカスラリーを効率よく製造する方法に関し、より詳しくは、石英粉を水等と混合し、撹拌混練してシリカスラリーを製造する方法において、凝集体の少ない均一なシリカスラリーを製造する方法に関する。 The present invention relates to a method for efficiently producing a uniform silica slurry with few aggregates, and more specifically, in a method for producing a silica slurry by mixing quartz powder with water or the like and stirring and kneading to produce a uniform silica slurry with little aggregates. The present invention relates to a method for producing a silica slurry.
石英粉を水等に混合して均一なスラリーを製造方法として、（イ）高圧ポンプを用いて石英粉と水等の混合流体をオリフィスに通過させて石英粉を分散させる方法（特許文献１）、（ロ）石英粉と水等の混合流体を相対向するノズルから噴射し、衝突させて粉砕し、分散させる方法（特許文献２）、多種類の混合装置を用いる方法（特許文献３）などが知られている。 As a method for producing a uniform slurry by mixing quartz powder with water, etc., (a) a method of dispersing quartz powder by passing a mixed fluid such as quartz powder and water through an orifice using a high-pressure pump (Patent Document 1). (B) A method in which a mixed fluid such as quartz powder and water is jetted from opposing nozzles, collided, pulverized, and dispersed (Patent Document 2), a method using various types of mixing devices (Patent Document 3), etc. It has been known.
シリカスラリーを製造する従来の上記方法は、何れも、石英粉を前処理せずに水等と混合して使用しているため、この混合物を撹拌混合して分散させ、あるいは噴射衝突させて分散させてスラリーを製造したときに、凝集体が多く分散性の劣るスラリーになる問題があった。 All of the above-mentioned conventional methods for producing silica slurry are used by mixing quartz powder with water or the like without pre-treatment, so this mixture is stirred and mixed or dispersed by jetting collision. When the slurry was produced, there was a problem that the slurry had many aggregates and poor dispersibility.
本発明は、石英と液体の混合体を撹拌混練してシリカスラリーを製造する方法において、予め調整した石英粉を用いることによって凝集体の少ない均一なシリカスラリーを製造する方法を提供する。 The present invention provides a method for producing a uniform silica slurry with few aggregates by using a silica powder prepared in advance by stirring and kneading a mixture of quartz and liquid.
本発明は以下の構成によって従来の課題を解決したシリカスラリーの製造方法に関する。
〔１〕表面に突片が設けられている回転盤を備えた混合槽に石英粉と液体の混合体を供給し、回転盤表面の突片によって石英粉と液体の混合体を撹拌混合してスラリーにする方法において、比表面積が３倍以上異なる石英粉を混合した混合石英粉を使用することによって凝集体の発生を抑制することを特徴とするシリカスラリーの製造方法。
〔２〕比表面積が３倍以上異なる石英粉を混合した比表面積７０〜１１０ｍ2/ｇの混合石英粉を用いる上記[１]に記載するシリカスラリーの製造方法。
〔３〕スラリー濃度３０〜４０wt％、および回転数５００〜２５００rpmにおいて、凝集体量を１.５wt％以下に抑制する上記[１]または上記[２]に記載するシリカスラリーの製造方法。
〔４〕スラリー濃度３０〜４０wt％、および回転数２５００〜３５００rpmにおいて、凝集体量を３.０wt％以下に抑制する上記[１]または上記[２]に記載するシリカスラリーの製造方法。
The present invention relates to a method for producing a silica slurry which has solved the conventional problems with the following constitution.
[1] A mixture of quartz powder and liquid is supplied to a mixing tank equipped with a rotating disk having protrusions on the surface, and the mixture of quartz powder and liquid is stirred and mixed by the protrusions on the surface of the rotating disk. In the method of making a slurry, a method for producing a silica slurry is characterized in that the generation of aggregates is suppressed by using mixed quartz powder in which quartz powder having a specific surface area different by 3 times or more is mixed.
[2] The method for producing a silica slurry as described in [1] above, wherein the mixed quartz powder having a specific surface area of 70 to 110 m 2 / g mixed with quartz powder having a specific surface area that is three times or more different is mixed.
[3] The method for producing a silica slurry according to the above [1] or [2], wherein the aggregate amount is suppressed to 1.5 wt% or less at a slurry concentration of 30 to 40 wt% and a rotation speed of 500 to 2500 rpm.
[4] The method for producing a silica slurry according to the above [1] or [2], wherein the aggregate amount is suppressed to 3.0 wt% or less at a slurry concentration of 30 to 40 wt% and a rotation speed of 2500 to 3500 rpm.
〔具体的な説明〕
以下、本発明を具体的に説明する。
本発明は、表面に突片が設けられている回転盤を備えた混合槽に石英粉と液体の混合体を供給し、回転盤表面の突片によって石英粉と液体の混合体を撹拌混合してスラリーにする方法において、比表面積が３倍以上異なる石英粉を混合した混合石英粉を使用することによって凝集体の発生を抑制することを特徴とするシリカスラリーの製造方法である。
[Specific description]
Hereinafter, the present invention will be specifically described.
The present invention supplies a mixture of quartz powder and liquid to a mixing tank equipped with a rotating disk having protrusions on the surface, and stirs and mixes the mixture of quartz powder and liquid with the protrusions on the surface of the rotating disk. In this method, the production of the silica slurry is characterized in that the generation of aggregates is suppressed by using mixed quartz powder in which quartz powders having different specific surface areas of three times or more are mixed.
表面に突片が設けられている回転盤を備えた混合槽に石英粉と液体の混合体を供給し、回転盤表面の突片によって石英粉と液体の混合体を撹拌混合してスラリーにする製造方法に用いる混練装置の一例を図１に示す。混合槽１０の内部に回転盤１１が混合槽１０の底部から離れて設置されている。該回転盤１１は回転軸１４によって回転自在に支持されており、該回転盤１１の表面に混合槽１０の底面に向かって複数の突片１２が同心円状に突き出している。図示する突片１２の大きさは長さ２〜３cmおよび表面積７〜１６cm2の円柱である。該突片１２の個数は回転盤直径２０〜３０cmの円形に対して２０〜４０個であればよい。また、混合槽１０の深さは回転盤１０の突片１２が混合槽底部から１〜５cm離れる程度であれば良い。なお、本発明の製造方法に用いる混練装置は図１の装置に限らない。表面に突片が設けられている回転盤を備えた混練装置であれば良い。
A mixture of quartz powder and liquid is supplied to a mixing tank equipped with a rotating disk having protrusions on the surface, and the mixture of quartz powder and liquid is stirred and mixed with the protrusions on the surface of the rotating disk to form a slurry. An example of a kneading apparatus used in the production method is shown in FIG. A rotating
石英粉と液体（主に水）の混合体は、回転盤１１の上面に供給され、回転盤１１の遠心力によって回転盤１１の外周に押し出され、回転盤外周と混合槽内壁の隙間から回転盤１１の下側に流れ込み、回転盤１１と混合槽底部の間に溜まる。この石英粉と液体の混合体は回転盤１１と一体に回動する突片１２によって撹拌混合されて石英粉が分散したスラリーになり、取り出し口１３を通じて外部に流出される。
A mixture of quartz powder and liquid (mainly water) is supplied to the upper surface of the
従来、図１の混練装置を用い、例えば、平均一次粒子径が１０ｎｍ〜２０ｎｍの石英粉と水の混合体を上記混練装置に供給して撹拌混練すると、混練初期には平均粒子径１０〜３０μmの凝集体が多数生じる。この凝集体は撹拌混練が進行すると次第に減少するが、従来の混練方法では、石英粉の６０wt％前後が凝集体として残り、石英粉が供給時の粒子径を維持して均一に分散したスラリーを得るのが難しい。 Conventionally, when a mixture of quartz powder and water having an average primary particle diameter of 10 nm to 20 nm is supplied to the above kneading apparatus and stirred and kneaded, for example, an average particle diameter of 10 to 30 μm is initially used. Many agglomerates are formed. This agglomerate gradually decreases as stirring and kneading progresses. However, in the conventional kneading method, about 60 wt% of the quartz powder remains as an agglomerate, and a slurry in which the quartz powder is uniformly dispersed while maintaining the particle size at the time of supply is obtained. Difficult to get.
そこで、石英粉と液体の混合体に接触する回転盤表面および突片表面の動摩擦係数と回転盤の回転数を所定の範囲に制御することによって凝集体の発生を抑制する方法が提案されている。具体的には、上記動摩擦係数を０.０５〜０.４の範囲に設定し、回転盤を５００rpm〜４０００rpm未満の回転数で回転することによって、原料の石英粉の二次粒子径よりも粒径の大きい凝集体の量が１０wt％以下であって、粘度２５０mPa・S以下のシリカスラリーを製造することが提案されている（特願２０１２−０８１６６４号）。 In view of this, a method has been proposed in which the generation of aggregates is controlled by controlling the dynamic friction coefficient of the surface of the rotating disk and the surface of the projecting piece contacting the mixture of quartz powder and liquid and the rotational speed of the rotating disk within a predetermined range. . Specifically, the dynamic friction coefficient is set in the range of 0.05 to 0.4, and the rotating disk is rotated at a rotational speed of 500 rpm to less than 4000 rpm, so that the particle diameter is larger than the secondary particle diameter of the raw material quartz powder. It has been proposed to produce a silica slurry having a large diameter aggregate of 10 wt% or less and a viscosity of 250 mPa · S or less (Japanese Patent Application No. 2012-081664).
本発明の製造方法は、石英と液体の混合体を撹拌混練してシリカスラリーを製造する方法において、動摩擦係数を一定範囲に設定する上記製造方法とは別に、比表面積が異なる石英粉を混合した石英粉を用いることによって凝集体の少ない均一なシリカスラリーを製造する方法である。 The production method of the present invention is a method for producing a silica slurry by stirring and kneading a mixture of quartz and liquid, and in addition to the above production method for setting a dynamic friction coefficient within a certain range, quartz powders having different specific surface areas are mixed. This is a method for producing a uniform silica slurry with few aggregates by using quartz powder.
具体的には、比表面積が３倍以上異なる石英粉を混合して用いる。例えば、比表面積５０ｍ2/ｇの石英粉と比表面積２００ｍ2/ｇの石英粉を混合し、混合後の比表面積が７０〜１１０ｍ2/ｇになるように混合量を調整した混合石英粉（混合石英粉Ｘ１：比表面積の比４倍）を用いると良い。また、比表面積５０ｍ2/ｇの石英粉と比表面積３００ｍ2/ｇの石英粉を混合し、混合後の比表面積が７０〜１１０ｍ2/ｇになるように混合量を調整した混合石英粉（混合石英粉Ｘ２：比表面積の比６倍）を用いると良い。 Specifically, quartz powders having different specific surface areas of 3 times or more are mixed and used. For example, a mixed quartz powder (a mixture of quartz powder having a specific surface area of 50 m 2 / g and quartz powder having a specific surface area of 200 m 2 / g and adjusting the mixing amount so that the specific surface area after mixing is 70 to 110 m 2 / g) Mixed quartz powder X1: ratio of specific surface area 4 times) may be used. Further, mixed quartz powder (mixed quartz powder having a specific surface area of 50 m 2 / g mixed with quartz powder having a specific surface area of 300 m 2 / g and adjusting the mixing amount so that the specific surface area after mixing is 70 to 110 m 2 / g ( Mixed quartz powder X2: 6 times the specific surface area) may be used.
上記混合石英粉Ｘ１、Ｘ２を用いれば、図１の混練装置（回転盤表面および突片表面の動摩擦係数０.１、以下、単に混練装置と云う）において、スラリー濃度３０〜４０wt％および回転数５００〜２０００rpmで、１０分間撹拌混合することによって、凝集体（粒径０.２μm以上の粒子）量１.５wt％以下のシリカスラリーを得ることができる。 When the mixed quartz powders X1 and X2 are used, in the kneading apparatus of FIG. 1 (coefficient of dynamic friction of the surface of the rotating disk and the surface of the protruding piece 0.1, hereinafter simply referred to as the kneading apparatus), the slurry concentration is 30 to 40 wt% and the rotational speed. By stirring and mixing at 500 to 2000 rpm for 10 minutes, a silica slurry having an aggregate (particles having a particle diameter of 0.2 μm or more) of 1.5 wt% or less can be obtained.
また、上記混合石英粉Ｘ１、Ｘ２を用いれば、上記混練装置において、スラリー濃度３０〜４０wt％および回転数２５００〜３５００rpmで、１０分間撹拌混合することによって、凝集体量３.０wt％以下のシリカスラリーを得ることができる。 In addition, when the mixed quartz powder X1 and X2 are used, in the above-mentioned kneading apparatus, by mixing with stirring at a slurry concentration of 30 to 40 wt% and a rotational speed of 2500 to 3500 rpm for 10 minutes, an aggregate amount of silica of 3.0 wt% or less is obtained. A slurry can be obtained.
一方、比表面積が単一の石英粉を用いると、凝集体の発生を十分に抑制することができない。例えば、比表面積（９０ｍ2/ｇ）が一種類の石英粉（石英粉Ｚ）を用いると、上記混練装置において、スラリー濃度３０〜４０wt％、５００rpm〜２０００rpmの回転数で、１０分間撹拌混練すると、スラリー中の凝集体量は３.０wt％（500rpm）、２.１wt％（2000rpm）であり、何れの場合も凝集体量は２.０wt％以上である。 On the other hand, when quartz powder having a single specific surface area is used, the generation of aggregates cannot be sufficiently suppressed. For example, when one kind of quartz powder (quartz powder Z) having a specific surface area (90 m 2 / g) is used, the mixture is stirred and kneaded for 10 minutes at a slurry concentration of 30 to 40 wt% and a rotation speed of 500 rpm to 2000 rpm in the kneading apparatus. The amount of aggregates in the slurry is 3.0 wt% (500 rpm) and 2.1 wt% (2000 rpm). In any case, the amount of aggregates is 2.0 wt% or more.
また上記石英粉Ｚを用いると、上記スラリー濃度（３０〜４０wt％）のとき、回転数２５００〜３５００rpmで同じ時間撹拌混練したとき、スラリー中の凝集体量は７.２wt％（3250rpm）であり、混合石英粉Ｘ１、Ｘ２を用いた場合に比べてスラリー中の凝集体量が格段に多い（約３倍以上）。 Further, when the quartz powder Z is used, when the slurry concentration is 30 to 40 wt%, the amount of agglomerates in the slurry is 7.2 wt% (3250 rpm) when the mixture is stirred and kneaded at the rotation speed of 2500 to 3500 rpm for the same time. The amount of agglomerates in the slurry is much larger (about 3 times or more) than when the mixed quartz powders X1 and X2 are used.
本発明はスラリー濃度４０〜５０wt％の場合も同様に適用することができる。例えば、上記混合石英粉Ｘ２を用いれば、上記混練装置において、スラリー濃度４０〜５０wt％および回転数５００〜２０００rpmで１０分間撹拌混合することによって、凝集体量０.２〜０.５wt％のシリカスラリーを得ることができる。 The present invention can be similarly applied to a slurry concentration of 40 to 50 wt%. For example, when the mixed quartz powder X2 is used, in the kneading apparatus, the mixture is stirred and mixed at a slurry concentration of 40 to 50 wt% and a rotation speed of 500 to 2000 rpm for 10 minutes, whereby an aggregate amount of 0.2 to 0.5 wt% is obtained. A slurry can be obtained.
一方、比表面積が一種類の石英粉Ｚを用いると、上記スラリー濃度（４０〜５０wt％）および上記回転数（５００〜２０００rpm）で同じ時間撹拌混合すると、スラリー中の凝集体量は０.８〜１.６wt％であり、混合石英粉Ｘ２を用いた場合に比べてスラリー中の凝集体量が格段に多い（約２倍〜８倍）。 On the other hand, when quartz powder Z having a single specific surface area is used, when the slurry concentration (40 to 50 wt%) and the rotational speed (500 to 2000 rpm) are stirred and mixed for the same time, the amount of aggregate in the slurry is 0.8. It is ˜1.6 wt%, and the amount of agglomerates in the slurry is much larger (about 2 to 8 times) than when the mixed quartz powder X2 is used.
回転数が２５００〜３５００rpmの場合も同様である。例えば、混合石英粉Ｘ２を用いれば、上記混練装置において、スラリー濃度４０〜５０wt％および回転数２５００〜３５００rpmで１０分間撹拌混合することによって凝集体量２.２〜２.３wt％のシリカスラリーを得ることができる。 The same applies when the rotational speed is 2500 to 3500 rpm. For example, when the mixed quartz powder X2 is used, a silica slurry having an aggregate amount of 2.2 to 2.3 wt% is obtained by stirring and mixing in the kneading apparatus at a slurry concentration of 40 to 50 wt% and a rotation speed of 2500 to 3500 rpm for 10 minutes. Can be obtained.
一方、石英粉Ｚを用いると、上記スラリー濃度（４０〜５０wt％）および上記回転数（２５００〜３５００rpm）で同じ時間撹拌混合すると、スラリー中の凝集体量は４.６wt％（3250rpm）であり、混合石英粉X２を用いた場合に比べてスラリー中の凝集体量が格段に多い（約２倍〜３倍）。 On the other hand, when quartz powder Z is used, the amount of aggregate in the slurry is 4.6 wt% (3250 rpm) when the slurry concentration (40 to 50 wt%) and the rotation speed (2500 to 3500 rpm) are stirred and mixed for the same time. The amount of agglomerates in the slurry is remarkably larger than when the mixed quartz powder X2 is used (about 2 to 3 times).
本発明の製造方法によれば、シリカスラリー中の凝集体の量を大幅に低減することができる。本発明の製造方法は、比表面積が３倍以上異なる石英粉を混合して用いればよく、従来の混練装置を使用することができるので実施が容易であり、しかも凝集体の量を低減する効果が優れている。 According to the production method of the present invention, the amount of aggregates in the silica slurry can be greatly reduced. The production method of the present invention only needs to be used by mixing quartz powder having a specific surface area that is three times or more different, and can be carried out easily because a conventional kneading apparatus can be used, and also has the effect of reducing the amount of aggregates. Is excellent.
以下、本発明の実施例を比較例と共に示す。
実施例および比較例において、石英粉は比表面積が示されている市販品（フュームドシリカ）を使用し、石英粉の混合は気流式混合機を用いた。混合石英粉の比表面積はQUANTACHROME社の測定機（AUTOSORB-iQ2型）を用いて測定した。なお、混合石英粉の比表面積は、比表面積ａ1m2/gの石英粉ｂ1ｇと比表面積ａ2m2/gの石英粉ｂ2ｇを混合したとき、〔(a1×b1)＋(a2×b2)〕／〔b1＋b2〕m2/gの式によって求められる。また、スラリーの粘度は東機産業社のＢ型粘度計(ＢＭII型)を用いて測定した。さらに、スラリー中の石英粉の粒子径を堀場製作所社のレーザ回折式粒度分布計(ＬＡ−９５０)を用いて測定し、粒子径が０.２μmを上回るものを凝集体としてその量を測定した。
Examples of the present invention are shown below together with comparative examples.
In the examples and comparative examples, the quartz powder used was a commercial product (fumed silica) with a specific surface area, and the quartz powder was mixed using an airflow mixer. The specific surface area of the mixed quartz powder was measured using a measuring machine (AUTOSORB-iQ2 type) manufactured by QUANTACHROME. The specific surface area of the mixed quartz powder, upon mixing the quartz powder b2g quartz powder b1g specific surface area a2m 2 / g of specific surface area of a1m 2 / g, [(a1 × b1) + (a2 × b2) ] / It is calculated | required by the formula of [b1 + b2] m < 2 > / g. The viscosity of the slurry was measured using a B-type viscometer (BMII type) manufactured by Toki Sangyo Co., Ltd. Furthermore, the particle diameter of the quartz powder in the slurry was measured using a laser diffraction particle size distribution analyzer (LA-950) manufactured by Horiba, Ltd., and the amount of the aggregate was measured with the particles having a particle diameter exceeding 0.2 μm as an aggregate. .
〔実施例１：A1〜A3〕
比表面積５０m2/gの石英粉と比表面積２００m2/gの二種の石英粉を混合し、比表面積が７０〜１１０m2/gになるように混合量を調整した。この混合石英粉X１（比表面積の比４倍）と純水を図１の混練装置に供給し、スラリー濃度３０〜４０wt％に調整し、回転盤の回転数を表１に示すように設定し、１０分間撹拌混練してシリカスラリーを製造した。このシリカスラリーの凝集体量および粘度を表１に示した。
[Example 1: A1 to A3]
The two kinds of silica powder of quartz powder and a specific surface area of 200 meters 2 / g of specific surface area of 50 m 2 / g were mixed, specific surface area was adjusted mixing amount such that the 70~110m 2 / g. This mixed quartz powder X1 (4 times the specific surface area ratio) and pure water are supplied to the kneading apparatus shown in FIG. 1, adjusted to a slurry concentration of 30 to 40 wt%, and the rotation speed of the rotating disk is set as shown in Table 1. A silica slurry was produced by stirring and kneading for 10 minutes. Table 1 shows the aggregate amount and viscosity of the silica slurry.
〔実施例２：A4〜A6〕
比表面積５０m2/gの石英粉と比表面積３００m2/gの二種の石英粉を混合し、比表面積が７０〜１１０m2/gになるように混合量を調整した。この混合石英粉X２（比表面積の比６倍）を用い、スラリー濃度３０〜４０wt％に調整し、回転盤の回転数を表１に示すように設定し、１０分間撹拌混練してシリカスラリーを製造した。このシリカスラリーの凝集体量および粘度を表１に示した。
[Example 2: A4 to A6]
The two kinds of silica powder of quartz powder and a specific surface area of 300 meters 2 / g of specific surface area of 50 m 2 / g were mixed, specific surface area was adjusted mixing amount such that the 70~110m 2 / g. Using this mixed quartz powder X2 (six times the specific surface area), adjusting the slurry concentration to 30 to 40 wt%, setting the rotation speed of the rotating disk as shown in Table 1, stirring and kneading for 10 minutes, Manufactured. Table 1 shows the aggregate amount and viscosity of the silica slurry.
〔実施例２：A7〜A9〕
上記混合石英粉X２（比表面積の比６倍）を用い、スラリー濃度４０〜５０wt％に調整し、回転盤の回転数を表１に示すように設定し、１０分間撹拌混練してシリカスラリーを製造した。このシリカスラリーの凝集体量および粘度を表１に示した。
[Example 2: A7 to A9]
Using the above mixed quartz powder X2 (six times the specific surface area), adjusting the slurry concentration to 40 to 50 wt%, setting the number of revolutions of the rotating disk as shown in Table 1, stirring and kneading for 10 minutes to obtain the silica slurry Manufactured. Table 1 shows the aggregate amount and viscosity of the silica slurry.
〔比較例１：B1〜B3〕
比表面積５０m2/gの石英粉と比表面積１２０m2/gの二種の石英粉を混合し、比表面積が７０〜１１０m2/gになるように混合量を調整した。この混合石英粉Y（比表面積の比２.４倍）を用い、スラリー濃度３０〜４０wt％に調整し、回転盤の回転数を表１に示すように設定し、１０分間撹拌混練してシリカスラリーを製造した。このシリカスラリーの凝集体量および粘度を表１に示した。
[Comparative Example 1: B1 to B3]
The two kinds of silica powder of quartz powder and a specific surface area of 120 m 2 / g of specific surface area of 50 m 2 / g were mixed, specific surface area was adjusted mixing amount such that the 70~110m 2 / g. Using this mixed quartz powder Y (2.4 times the specific surface area ratio), adjusting the slurry concentration to 30 to 40 wt%, setting the rotation speed of the rotating disk as shown in Table 1, stirring and kneading for 10 minutes to silica A slurry was produced. Table 1 shows the aggregate amount and viscosity of the silica slurry.
〔比較例１：B4〜B9〕
比表面積９０m2/gの石英粉を一種類用い、スラリー濃度３０〜５０wt％に調整し、回転盤の回転数を表１に示すように設定し、１０分間撹拌混練してシリカスラリーを製造した。このシリカスラリーの凝集体量および粘度を表１に示した。
[Comparative Example 1: B4 to B9]
Using one kind of quartz powder with a specific surface area of 90 m 2 / g, adjusting the slurry concentration to 30-50 wt%, setting the rotation speed of the rotating disk as shown in Table 1, and stirring and kneading for 10 minutes to produce a silica slurry. . Table 1 shows the aggregate amount and viscosity of the silica slurry.
実施例１〜２の試料No.A1、A2、A4、A5は、スラリー濃度３０〜４０wt％および回転数５００〜２０００rpmにおいて、凝集体量１.５wt％以下であり、凝集体量の少ないシリカスラリーが得られる。また、試料No.A3、A6は回転数が３２５０rpmでも凝集体量は３.０wt％以下である。 Samples Nos. A1, A2, A4, and A5 of Examples 1 and 2 are silica slurries having a small aggregate amount with an aggregate amount of 1.5 wt% or less at a slurry concentration of 30 to 40 wt% and a rotational speed of 500 to 2000 rpm. Is obtained. Sample Nos. A3 and A6 have an aggregate amount of 3.0 wt% or less even at a rotational speed of 3250 rpm.
さらに、実施例３の試料No.A7、A8は、スラリー濃度４０〜５０wt％および回転数５００〜２０００rpmにおいて、凝集体量０.５wt％以下であり、凝集体量が格段に少ないシリカスラリーが得られる。 Further, Sample Nos. A7 and A8 of Example 3 have a silica concentration with an agglomerate amount of 0.5 wt% or less at a slurry concentration of 40 to 50 wt% and a rotation speed of 500 to 2000 rpm, and a silica slurry with a remarkably small amount of agglomerate is obtained. It is done.
一方、比較例１の試料（No.B1〜B3）は、混合石英粉の比表面積の比が３倍以下（２.４倍）であるため、シリカスラリー中の凝集量は、回転数５００〜２０００rpmにおいて２.１〜３.３wt％であり、実施例１〜２の試料No.A1、A2、A4、A5より凝集体の量が多い。また、回転数３２５０rpmにおいて凝集体の量は６.８〜７.５wt％であり、実施例１〜３の試料（No.A3,A6,A9）より凝集体量が多い。 On the other hand, since the sample of Comparative Example 1 (No. B1 to B3) has a specific surface area ratio of the mixed quartz powder of 3 times or less (2.4 times), the amount of aggregation in the silica slurry is 500 to 500 rpm. It is 2.1 to 3.3 wt% at 2000 rpm, and the amount of aggregate is larger than those of Sample Nos. A1, A2, A4, and A5 of Examples 1-2. Moreover, the amount of aggregates is 6.8 to 7.5 wt% at a rotational speed of 3250 rpm, and the amount of aggregates is larger than the samples of Examples 1 to 3 (No. A3, A6, A9).
比較例２の試料（No.B4〜B6）は、比表面積が一種類の石英粉を用いているので、スラリー濃度３０〜４０wt％および回転数５００〜３２５０rpmにおいて、何れも実施例１〜２の試料No.A1〜A6より凝集体量が格段に多い。 Since the sample (No. B4 to B6) of Comparative Example 2 uses one kind of quartz powder having a specific surface area, each of Examples 1 and 2 is used at a slurry concentration of 30 to 40 wt% and a rotation speed of 500 to 3250 rpm. The amount of aggregates is much higher than Sample Nos. A1 to A6.
比較例３の試料（No.B7,B8）は、スラリー濃度４０〜５０wt％のとき、回転数５００〜２０００rpmにおいて凝集体の量は０.８〜１.６wt％であり、同様のスラリー濃度および回転数の実施例試料（No.A7,A8）より凝集体量が多い。また、試料No.B9は回転数３２５０rpmにおいて凝集体量４.６wt％であり、同様のスラリー濃度および回転数の実施例試料（No.A9）より凝集体量が格段に多い。 The samples of Comparative Example 3 (No. B7, B8) had a slurry concentration of 0.8 to 1.6 wt% at a rotation speed of 500 to 2000 rpm when the slurry concentration was 40 to 50 wt%. The amount of aggregate is larger than that of the sample samples (No. A7, A8) of the number of rotations. Sample No. B9 has an aggregate amount of 4.6 wt% at a rotational speed of 3250 rpm, and the amount of aggregate is much larger than that of the example sample (No. A9) having the same slurry concentration and rotational speed.
１０−混合槽、１１−回転盤、１２−突片、１３−取出口、１４−回転軸。 10-mixing tank, 11-rotary disc, 12-projection piece, 13-outlet, 14-rotating shaft.
Claims (4)
A mixture of quartz powder and liquid is supplied to a mixing tank equipped with a rotating disk having protrusions on the surface, and the mixture of quartz powder and liquid is stirred and mixed with the protrusions on the surface of the rotating disk to form a slurry. A method for producing a silica slurry, characterized in that in the method, the generation of aggregates is suppressed by using mixed quartz powder in which quartz powders having specific surface areas different by 3 times or more are mixed.
The method for producing a silica slurry according to claim 1, wherein mixed silica powder having a specific surface area of 70 to 110 m 2 / g mixed with quartz powder having a specific surface area that is three or more times different is used.
The method for producing a silica slurry according to claim 1 or 2, wherein the amount of aggregates is suppressed to 1.5 wt% or less at a slurry concentration of 30 to 40 wt% and a rotational speed of 500 to 2500 rpm.
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| US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
| US11236002B2 (en) | 2015-12-18 | 2022-02-01 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of an opaque quartz glass body |
| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
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| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
| US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
| US11708290B2 (en) | 2015-12-18 | 2023-07-25 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
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- 2012-10-31 JP JP2012240482A patent/JP2014088298A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
| US11236002B2 (en) | 2015-12-18 | 2022-02-01 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of an opaque quartz glass body |
| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
| US11339076B2 (en) | 2015-12-18 | 2022-05-24 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of carbon-doped silicon dioxide granulate as an intermediate in the preparation of quartz glass |
| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
| US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
| US11708290B2 (en) | 2015-12-18 | 2023-07-25 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
| US11952303B2 (en) | 2015-12-18 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Increase in silicon content in the preparation of quartz glass |
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