JP5749485B2 - Alumina fiber pulverized product, method for producing the same, and resin composition using the same - Google Patents
Alumina fiber pulverized product, method for producing the same, and resin composition using the same Download PDFInfo
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本発明は、アルミナ質繊維粉砕品及びその製造方法、並びにそれを用いた樹脂組成物用に関する。 The present invention relates to an alumina fiber pulverized product, a method for producing the same, and a resin composition using the same.
アルミナ質繊維集合体の繊維長を制御する方法は、繊維集合体をロールミルやプレス機等で粉砕する方法が知られているが、繊維長分布がブロードとなる問題点があった。この問題を解決するため、一度粉砕した集合体を気流分級装置などで分級処理する方法が検討されている（特許文献１）。しかしながら、得られる集合体の収率が低いという問題点があった。 As a method for controlling the fiber length of the alumina fiber assembly, a method of pulverizing the fiber assembly with a roll mill or a press machine is known, but there is a problem that the fiber length distribution becomes broad. In order to solve this problem, a method of classifying an aggregate once pulverized with an airflow classifier or the like has been studied (Patent Document 1). However, there is a problem that the yield of the obtained aggregate is low.
こぶ状のふくらみを有する繊維の製造方法としては、Ａｌ２Ｏ３とＳｉＯ２を主成分とする組成物を溶融させる方法（特許文献２）がある。また、塩基性アルミニウム溶液とコロイド状シリカと有機重合体を含む紡糸原液をノズルから吐出させ、前駆体繊維を得て、これを焼成する方法（特許文献３）等が知られている。 As a method for producing a fiber having a knurled bulge, there is a method (Patent Document 2) in which a composition mainly composed of Al 2 O 3 and SiO 2 is melted. Also known is a method (Patent Document 3) or the like in which a spinning solution containing a basic aluminum solution, colloidal silica, and an organic polymer is discharged from a nozzle to obtain a precursor fiber, which is fired.
本発明は、繊維長分布が制御されたアルミナ質繊維粉砕品、及びその粉砕品が容易に得られる製造方法、並びにそれを用いた樹脂組成物を提供することである。 An object of the present invention is to provide an alumina fiber pulverized product having a controlled fiber length distribution, a production method for easily obtaining the pulverized product, and a resin composition using the same.
本発明は、（１）ネッキングを有したアルミナ質繊維集合体を粉砕してなる、繊維長の変動係数が１０％以下であるアルミナ質繊維粉砕品、（２）ネッキングの間隔が１０〜１５０μｍであるアルミナ質繊維集合体を用いる（１）のアルミナ質繊維粉砕品、（３）粉砕をプレス圧力０．１〜２０ＭＰａで行う（１）又は（２）のアルミナ質繊維粉砕品の製造方法、（４）プレスの加圧速度が０．５〜５ＭＰａ／秒である（３）のアルミナ質繊維粉砕品の製造方法、（５）圧力の保持時間が３０秒以下である（３）又は（４）のアルミナ質繊維粉砕品の製造方法、（６）（１）又は（２）のアルミナ質繊維粉砕品を含有してなる樹脂組成物、である。 The present invention includes (1) an alumina fiber pulverized product having a coefficient of variation of fiber length of 10% or less, obtained by pulverizing an alumina fiber assembly having necking, and (2) an interval between necking of 10 to 150 μm. alumina fiber pulverized products with an alumina fiber aggregate (1), (3) performing pulverizng a press pressure 0.1 to 20 MPa (1) or (2) aluminous method for producing fibers pulverized product of, ( 4 ) The method for producing an alumina fiber pulverized product according to ( 3 ), wherein the pressurization speed is 0.5 to 5 MPa / second, ( 5 ) the pressure holding time is 30 seconds or less ( 3 ) or ( 4 ), And a resin composition comprising the pulverized alumina fiber product of ( 6 ) (1) or (2) .
本発明によれば、繊維長分布が制御されたアルミナ質繊維粉砕品が容易に得られる。また、本発明のアルミナ質繊維粉砕品を使用すると良好な物性の樹脂組成物が得られる。 According to the present invention, an alumina fiber pulverized product having a controlled fiber length distribution can be easily obtained. Moreover, when the alumina fiber pulverized product of the present invention is used, a resin composition having good physical properties can be obtained.
本発明でいうネッキングを有するアルミナ質繊維集合体とは、１本のアルミナ質繊維において繊維径が太い部分と細い部分(ネッキング部分)が連続的に、かつ繊維全体にわたって存在し、太い部分の直径を１００とすると、ネッキング部分の直径が９０以下となっている繊維のことである。つまり、繊維径が太い部分（図１の１)と繊維径が細いネッキング部（図１の２)が繊維全体にわたり連続している繊維である。
本発明で言うネッキング間隔とはネッキング部で繊維径が最も小さい部分から隣り合うネック部の繊維径が最も小さい部分までの距離(図１の３)のことを言う。
The alumina fiber aggregate having necking as used in the present invention means that one alumina fiber has a thick fiber portion and a thin portion (necking portion) continuously and over the entire fiber, and the diameter of the thick portion. Is 100, the diameter of the necking portion is 90 or less. That is, it is a fiber in which a portion having a large fiber diameter (1 in FIG. 1) and a necking portion having a small fiber diameter (2 in FIG. 1) are continuous over the entire fiber.
The necking interval referred to in the present invention means a distance (3 in FIG. 1) from a portion having the smallest fiber diameter in the necking portion to a portion having the smallest fiber diameter in the adjacent neck portion.
この特定の間隔のネッキングを有するアルミナ質繊維集合体は、特に製造方法は限定されないが、例えば、以下の方法で製造することが可能である。
（１）塩基性塩化アルミニウムをＡｌ２Ｏ３換算で２５〜３５質量％、シリカゾルをＳｉＯ２換算で１〜１０質量%、ポリビニルアルコールを２〜３．５質量％、ポリエチレングリコールを０．２〜１．８質量％を含み、２０℃における粘度が１５００〜６０００ｍＰａ・ｓの水溶液を調製する工程
（２）上記水溶液を紡糸原液として、回転する中空円盤の側壁に設けられた複数個の細孔から吐出させて液糸化し前駆体繊維とする工程
（３）上記前駆体繊維を集めて焼成した後冷却する工程
を経て、製造することが可能である。
The production method of the alumina fiber aggregate having necking at a specific interval is not particularly limited, but can be produced by the following method, for example.
(1) 25 to 35% by mass of basic aluminum chloride in terms of Al 2 O 3 , 1 to 10% by mass of silica sol in terms of SiO 2, 2 to 3.5% by mass of polyvinyl alcohol, 0.2 to 0.2% of polyethylene glycol Step of preparing an aqueous solution containing 1.8% by mass and having a viscosity at 20 ° C. of 1500 to 6000 mPa · s (2) Using the aqueous solution as a spinning stock solution, a plurality of pores provided on the side wall of the rotating hollow disk It can be manufactured through a step of discharging and liquefying into precursor fibers (3) a step of collecting and firing the precursor fibers and then cooling.
ネッキング間隔の制御は、紡糸原液中のポリビニルアルコールとポリエチレングリコールの質量比などを変えることで制御が可能である。
ポリビニルアルコールは重合度が１０００〜５０００であることが好ましく、ポリエチレングリコールは分子量が３００〜１０００であることが好ましく、ポリビニルアルコール：ポリエチレングリコールの質量比が１：０．１０〜０．５であることが好ましい。
The necking interval can be controlled by changing the mass ratio of polyvinyl alcohol and polyethylene glycol in the spinning dope.
Polyvinyl alcohol preferably has a degree of polymerization of 1000 to 5000, polyethylene glycol preferably has a molecular weight of 300 to 1000, and a mass ratio of polyvinyl alcohol: polyethylene glycol is 1: 0.10 to 0.5. Is preferred.
本発明は、ネッキングを有するアルミナ質繊維集合体を粉砕することにより得られるアルミナ質繊維粉砕品である。ネッキングの間隔が１０〜１５０μｍであるアルミナ質繊維集合体を用いることが好ましく、このことにより、アルミナ質繊維粉砕品の平均繊維長を１０〜１５０μｍとすることが可能となる。
平均繊維長が１０μｍより小さいと樹脂と複合化したとき、充分な補強効果が得られず、１５０μｍを超えると分散性が悪化し、樹脂と均一に混合することが困難となる。また、繊維長の分布がブロードであると均一な補強効果が得られ難くなるため、繊維長の変動係数は１０％以下が好ましい。
ネッキングを有するアルミナ質繊維集合体は、繊維径が太い部分に比べ、ネッキング部分の強度が弱い為、圧力をかけると、ネッキング部分から選択的に折れる。その結果、粉砕されたネッキングを有するアルミナ質繊維粉砕品の繊維長は、ほぼネッキング間隔と等しく制御される。
The present invention is an alumina fiber pulverized product obtained by pulverizing an alumina fiber assembly having necking. It is preferable to use an alumina fiber aggregate having a necking interval of 10 to 150 μm, and this enables the average fiber length of the alumina fiber pulverized product to be 10 to 150 μm.
When the average fiber length is less than 10 μm, a sufficient reinforcing effect cannot be obtained when it is combined with the resin, and when it exceeds 150 μm, the dispersibility is deteriorated and it becomes difficult to uniformly mix with the resin. Further, if the fiber length distribution is broad, it is difficult to obtain a uniform reinforcing effect, and therefore the fiber length variation coefficient is preferably 10% or less.
Aluminous fiber aggregates having necking are selectively broken from the necking portion when pressure is applied because the strength of the necking portion is weaker than that of the portion having a large fiber diameter. As a result, the fiber length of the alumina fiber pulverized product having the pulverized necking is controlled to be substantially equal to the necking interval.
本発明のネッキングを有するアルミナ質繊維集合体の粉砕には、プレス粉砕機、ボールミル、攪拌粉砕器、ロールクラッシャーなどを用いることが出来るが、本発明は、プレスで粉砕する方法が好適に使用される。
プレス粉砕とは上下のプレス板の間に原料を投入し上下から圧力を加えて粉砕する方法である。市販品を例示すれば、三庄インダストリー社製商品名「テーブルプレス」、「ロータリープレス」、エヌピーシステム社商品名「ニュートンプレス」などである。
A press pulverizer, a ball mill, a stirring pulverizer, a roll crusher, or the like can be used for pulverizing the alumina fiber aggregate having the necking of the present invention. In the present invention, a method of pulverizing with a press is preferably used. The
Press pulverization is a method in which raw materials are put between upper and lower press plates and pulverized by applying pressure from above and below. Examples of commercially available products include “Table Press”, “Rotary Press”, and “Newton Press” manufactured by NP Systems Co., Ltd.
プレス圧力は０．１〜２０ＭＰａが好ましく、より好ましくは１〜１０ＭＰａである。圧力が０．１ＭＰａ未満では粉砕が不十分となり、ネック部分で粉砕されない繊維が発生し、繊維長分布がブロードになる場合がある。２０ＭＰａを超えると、繊維は通常の部分も粉砕され、所望の繊維長分布より短くなる場合がある。 The pressing pressure is preferably from 0.1 to 20 MPa, more preferably from 1 to 10 MPa. If the pressure is less than 0.1 MPa, pulverization becomes insufficient, and fibers that are not pulverized are generated at the neck portion, and the fiber length distribution may become broad. If the pressure exceeds 20 MPa, the normal part of the fiber may be pulverized and may be shorter than the desired fiber length distribution.
プレスの加圧速度は０．５〜５ＭＰａ／秒が好ましい。加圧速度が０．５ＭＰａより小さいと粉砕に必要以上に時間がかかり、５ＭＰａより大きいと急激な加圧により粉砕ムラが発生する場合がある。 The pressurization speed of the press is preferably 0.5 to 5 MPa / second. If the pressurization speed is less than 0.5 MPa, it takes more time than necessary for pulverization, and if it is greater than 5 MPa, pulverization unevenness may occur due to rapid pressurization.
プレスの最高圧力での保持時間は３０秒以下であることが好ましい。保持時間が長すぎると所望の繊維長より短くなりすぎる場合がある。より好ましい保持時間は５〜２０秒である。 The holding time at the maximum pressure of the press is preferably 30 seconds or less. If the holding time is too long, it may be shorter than the desired fiber length. A more preferable holding time is 5 to 20 seconds.
粉砕された繊維の繊維長分布は、市販の粒度・形状分布測定装置（例えば、株式会社セイシン企業社製ＰＩＴＡ−１）を用いて測定することができる。粒度・形状測定装置により、水を分散媒として用いて、任意の３０００本の繊維長を測定し、その平均値（平均繊維長）と標準偏差を求め、変動係数を以下の式（１）より計算した。なお、繊維長とは、測定繊維の任意の２点間の距離の最大長である。
変動係数（％）＝標準偏差／平均繊維長×１００
The fiber length distribution of the pulverized fibers can be measured using a commercially available particle size / shape distribution measuring apparatus (for example, PITA-1 manufactured by Seishin Enterprise Co., Ltd.). Using a particle size / shape measuring device, water is used as a dispersion medium to measure an arbitrary 3000 fiber lengths, an average value (average fiber length) and a standard deviation are obtained, and a coefficient of variation is obtained from the following equation (1). Calculated. The fiber length is the maximum length of the distance between any two points on the measurement fiber.
Coefficient of variation (%) = standard deviation / average fiber length × 100
本発明の繊維長が制御されたアルミナ質繊維粉砕品を樹脂組成物と複合化させる場合、樹脂組成は、特に限定されないが、エポキシ、アクリル、フェノール等の樹脂が好適である。 When the pulverized alumina fiber having a controlled fiber length according to the present invention is combined with the resin composition, the resin composition is not particularly limited, but resins such as epoxy, acrylic, and phenol are suitable.
「実験例１」
Ａｌ２Ｏ３濃度が２３．５質量％のオキシ塩化アルミニウム水溶液４７８３ｇとＳｉＯ２濃度が２１．０質量％のシリカゾル１３１０ｇ、重合度１７００のポリビニルアルコールの水溶液（濃度１０質量％）１１００ｇ、分子量６００のポリエチレングリコール１８ｇを混合してから減圧濃縮し、粘度３５００ｍＰａ・ｓの紡糸原液を調製した。濃縮後の紡糸原液はＡｌ２Ｏ３換算の含有率が２９．６質量％、ＳｉＯ２換算の含有率が７．４質量％、ポリビニルアルコールが２．８質量％、ポリエチレングリコールが０．４９質量％であった（ポリビニルアルコール：ポリエチレングリコールの質量比が１：０．１６）。
この紡糸原液を、回転する直径３５０ｍｍの中空円盤の側壁に設けられた直径０．２ｍｍ（細孔間隔：３．５ｍｍ）から吐出させて液糸化し、２００℃の熱風に浮遊させて乾燥させながら、下部から吸引する方式の集綿室に搬送し前駆体繊維を集積した。これを、ローラーハウス炉を用い大気雰囲気下で焼成した。焼成は、雰囲気温度が１０００℃までを１０℃／分で昇温し、１０００℃をこえ１２００℃までを１５℃／分の速度で昇温し、１２００℃で３０分間保持して行った。得られたアルミナ短繊維集合体のネッキング間隔は６０μｍであった。
得られたネッキングを有するアルミナ質繊維集合体を、内径８ｃｍ、深さが２０ｃｍの鋼製モールドに１００ｇ投入し、１０ＭＰａでプレス粉砕した。なお、加圧速度は３ＭＰａ／秒とし、最高圧力で１５秒間保持した。得られたアルミナ質繊維粉砕品の物性を表１に示す。
"Experiment 1"
4783 g of an aluminum oxychloride aqueous solution having an Al 2 O 3 concentration of 23.5% by mass, 1310 g of silica sol having an SiO 2 concentration of 21.0% by mass, 1100 g of an aqueous solution of polyvinyl alcohol having a polymerization degree of 1700 (concentration of 10% by mass), having a molecular weight of 600 After mixing 18 g of polyethylene glycol, the mixture was concentrated under reduced pressure to prepare a spinning dope having a viscosity of 3500 mPa · s. The concentrated spinning solution has an Al 2 O 3 content of 29.6% by mass, an SiO 2 content of 7.4% by mass, polyvinyl alcohol 2.8% by mass, and polyethylene glycol 0.49% by mass. % (The mass ratio of polyvinyl alcohol: polyethylene glycol was 1: 0.16).
This spinning dope is discharged from a diameter of 0.2 mm (pore spacing: 3.5 mm) provided on the side wall of a rotating hollow disk having a diameter of 350 mm to form a liquid yarn, suspended in hot air at 200 ° C. and dried. Then, it was conveyed to a cotton collection chamber using a suction method from the bottom, and the precursor fibers were accumulated. This was fired in an air atmosphere using a roller house furnace. Firing was performed by raising the temperature up to 1000 ° C. at 10 ° C./min, raising the temperature from 1000 ° C. to 1200 ° C. at a rate of 15 ° C./min, and holding at 1200 ° C. for 30 minutes. The necking interval of the obtained alumina short fiber aggregate was 60 μm.
100 g of the obtained alumina fiber assembly having necking was put into a steel mold having an inner diameter of 8 cm and a depth of 20 cm, and press-pulverized at 10 MPa. The pressurization rate was 3 MPa / second and the maximum pressure was maintained for 15 seconds. The physical properties of the obtained alumina fiber pulverized product are shown in Table 1.
［使用材料］
ポリビニルアルコール：電気化学工業株式会社製、デンカポバール、Ｂ−１７
ポリエチレングリコール：和光純薬工業株式会社製、試薬、ポリエチレングリコール６００
オキシ塩化アルミニウム：多木化学株式会社製、タキバイン、＃１５００
[Materials used]
Polyvinyl alcohol: Denka Poval, B-17, manufactured by Denki Kagaku Kogyo Co., Ltd.
Polyethylene glycol: Wako Pure Chemical Industries, Ltd., reagent, polyethylene glycol 600
Aluminum oxychloride: manufactured by Taki Chemical Co., Ltd., Takibine, # 1500
「実験例２」
ネッキング間隔を変える為、ポリビニルアルコールとポリエチレングリコールの質量比を変え、ネッキング間隔が異なるアルミナ質繊維集合体を製造した。これらの繊維集合体を用いたこと以外は実験例１と同様にアルミナ質繊維粉砕品を製造した。また、比較として、ネッキングのないアルミナ質繊維（電気化学工業社製商品名「デンカアルセンＢ８０Ｌ」アルミナ８０質量％、シリカ２０質量％）を粉砕しアルミナ質繊維粉砕品を製造した。得られたアルミナ質繊維粉砕品の物性を表２に示す。
"Experimental example 2"
In order to change the necking interval, the mass ratio of polyvinyl alcohol and polyethylene glycol was changed to produce alumina fiber assemblies having different necking intervals. An alumina fiber pulverized product was produced in the same manner as in Experimental Example 1 except that these fiber assemblies were used. As a comparison, alumina fiber without a necking (trade name “Denka Alsene B80L” alumina 80 mass%, silica 20 mass% manufactured by Denki Kagaku Kogyo Co., Ltd.) was pulverized to produce an alumina fiber pulverized product. Table 2 shows the physical properties of the obtained pulverized alumina fiber.
「実験例３」
プレス圧力、加圧速度、最高圧力での保持時間等のプレス条件を変えたこと以外は実験例１と同様にアルミナ質繊維粉砕品を製造した。得られたアルミナ質繊維粉砕品の物性を表３に示す。
"Experiment 3"
An alumina fiber pulverized product was produced in the same manner as in Experimental Example 1 except that the pressing conditions such as the pressing pressure, the pressing speed, and the holding time at the maximum pressure were changed. Table 3 shows the physical properties of the obtained pulverized alumina fiber.
表３より、プレス圧力、加圧速度、最高圧力での保持時間を適正化することにより、平均繊維長が制御され、標準偏差が小さく、変動係数の小さいアルミナ質繊維粉砕品が得られることが分かる。 From Table 3, by optimizing the holding time at the pressing pressure, pressing speed, and maximum pressure, it is possible to obtain an alumina fiber pulverized product in which the average fiber length is controlled, the standard deviation is small, and the coefficient of variation is small. I understand.
「実験例４」
実験例１で得られたアルミナ質繊維粉砕品と、市販されているネッキングのないアルミナ質繊維（電気化学工業社製商品名「デンカアルセンＢ８０Ｌ」アルミナ８０質量％、シリカ２０質量％）を実験Ｎｏ．１−１の条件にて粉砕した繊維を各々下記に示す配合割合で各材料を計量し、ビニール袋中でドライブレンドした後、ロール表面温度１００℃のミキシングロールを用いて５分間混練を行い、冷却粉砕した。粉砕品をトランスファー成型機（温度１７５℃、トランスファー出力５．１ＭＰａ、成型時間９０秒）で直径２８ｍｍ、厚さ３ｍｍの円板状のエポキシ樹脂硬化体を製造し、熱伝導率測定装置（アグネ社製「ＡＲＴ−ＴＣ−１型」）を用い測定環境温度２３℃で温度傾斜法にて熱伝導率を測定した。その結果を表４に示す。
"Experimental example 4"
Experiment No. 1 was obtained by pulverizing the alumina fiber obtained in Experimental Example 1 and a commercially available alumina fiber without necking (trade name “Denka Arsen B80L” alumina 80 mass%, silica 20 mass%, manufactured by Denki Kagaku Kogyo Co., Ltd.). . Each material was weighed at the following mixing ratios of the fibers pulverized under the conditions of 1-1, dry blended in a plastic bag, and then kneaded for 5 minutes using a mixing roll having a roll surface temperature of 100 ° C. Cooled and crushed. A crushed product is produced by a transfer molding machine (temperature: 175 ° C., transfer output: 5.1 MPa, molding time: 90 seconds) to produce a disk-shaped epoxy resin cured body having a diameter of 28 mm and a thickness of 3 mm. The thermal conductivity was measured by a temperature gradient method at a measurement environmental temperature of 23 ° C. using “ART-TC-1 type” manufactured by the manufacturer. The results are shown in Table 4.
［使用材料と配合割合］
アルミナ繊維粉砕品：２１４．７ｇ
アミノ系シランカップリング剤：１．２ｇ（信越化学工業社製商品名「ＫＢＥ−９０３」）
エポキシ樹脂：３７．２ｇ（ジャパンエポキシレジン社製商品名「ＹＸ−４０００Ｈ」）
エポキシ樹脂：１７．１ｇ（日本化薬社製商品名「ＥＣＯＮ−１０２０」）
硬化剤：２８．３ｇ（群栄化学工業社製商品名「ＰＳＭ−４２６１」）
ワックス：１．９ｇ（クラリアントジャパン社製商品名「ＷＡＸ−Ｅ」）
硬化促進剤：０．７ｇ（北興化学工業社製商品名「ＴＰＰ」）
[Use materials and blending ratio]
Alumina fiber pulverized product: 214.7 g
Amino-based silane coupling agent: 1.2 g (trade name “KBE-903” manufactured by Shin-Etsu Chemical Co., Ltd.)
Epoxy resin: 37.2 g (trade name “YX-4000H” manufactured by Japan Epoxy Resin Co., Ltd.)
Epoxy resin: 17.1 g (trade name “ECON-1020” manufactured by Nippon Kayaku Co., Ltd.)
Curing agent: 28.3 g (trade name “PSM-4261” manufactured by Gunei Chemical Industry Co., Ltd.)
Wax: 1.9 g (trade name “WAX-E” manufactured by Clariant Japan)
Curing accelerator: 0.7 g (trade name “TPP” manufactured by Hokuko Chemical Co., Ltd.)
表４より、本発明のアルミナ質繊維粉砕品を使用することにより、熱伝導率の高い樹脂組成物が得られることが分かる。 From Table 4, it can be seen that a resin composition having high thermal conductivity can be obtained by using the pulverized alumina fiber of the present invention.
本発明のネッキングを有したアルミナ質繊維集合体を用いて粉砕することで得られるアルミナ質繊維粉砕品は、例えば、高熱伝導用の樹脂組成物等のフィラーとして広範に使用することが出来る。 The alumina fiber pulverized product obtained by pulverizing using the alumina fiber aggregate having the necking of the present invention can be widely used as a filler for, for example, a resin composition for high thermal conductivity.
１：太い部分
２：ネッキング部
３：ネッキング間隔
1: Thick part 2: Necking part 3: Necking interval
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