JP4241424B2 - Boron nitride powder and mold release agent - Google Patents
Boron nitride powder and mold release agent Download PDFInfo
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Description
本発明は、窒化硼素粉末及びその水分散体からなる離型剤に関する。 The present invention relates to a release agent comprising boron nitride powder and an aqueous dispersion thereof.
窒化硼素（以下、「ＢＮ」ともいう。）粉末は、その良熱伝導性、低熱膨張性、溶融金属や溶融ガラスに濡れ難い耐食性等の性質を利用し、ガラス成型、アルミダイキャストの離型剤などに用いられている。しかしながら、ＢＮ粉末は疎水性が強いので離型剤とするには非水系の非極性溶媒に分散させるか、又は水分散体とするにしても、特許文献１のように多種の添加剤と処理工程が必要であった。 Boron nitride (hereinafter also referred to as “BN”) powder uses its properties such as good thermal conductivity, low thermal expansibility, and corrosion resistance that makes it difficult to get wet with molten metal and molten glass. It is used for agents. However, since BN powder is highly hydrophobic, it can be dispersed in a non-aqueous non-polar solvent or a water dispersion to form a release agent. A process was required.
一方、ＢＮ粉末のシランカップリング剤による表面処理として、特許文献２がある。ＢＮ粒子は、六方晶構造を有し、厚み（ｃ軸）方向の長さに対する幅（ａ軸）方向の長さの比で表される扁平度の値が小さい鱗片粒子であり、しかもＯＨ基はｃ軸方向にしか存在しない構造である。そのため、シランカップリング剤で処理をしても、シランカップリング剤はＢＮ粒子表面のＯＨ基にしか付着しないので十分な効果は得られず、その結果、非水系溶媒中への分散性は改良できても水に対する大幅な改善はなく、しかも得られた水分散体は泡立つので、その塗布面は凹凸となり離型性が低下した。
本発明の目的は、水分散性に優れ、消泡性に優れた水分散体を得ることができる窒化硼素粉末と、その水分散体からなる離型剤を提供することである。 An object of the present invention is to provide a boron nitride powder capable of obtaining an aqueous dispersion excellent in water dispersibility and excellent defoaming property, and a mold release agent comprising the aqueous dispersion.
すなわち、本発明は、メトキシ基と、ポリエチレングリコール及びポリプロピレングリコールユニットからなる官能基とを有する分子量２５０以上のシランカップリング剤で処理されてなる、シランカップリング剤の含有率が０．５〜１０質量％の窒化硼素粉末を用いた、水分散体中の窒化硼素粉末が１〜３０質量％であることを特徴とする離型剤である。 That is, the present invention has a silane coupling agent content of 0.5 to 10 which is treated with a silane coupling agent having a methoxy group and a functional group composed of polyethylene glycol and polypropylene glycol units and having a molecular weight of 250 or more. A release agent characterized in that the boron nitride powder in an aqueous dispersion is 1 to 30% by mass using a mass% boron nitride powder .
本発明によれば、水分散性に優れたＢＮ粉末が得られる。また、泡立ちによる離型性が損なわれない水性の離型剤が得られる。 According to the present invention, a BN powder excellent in water dispersibility can be obtained. Moreover, the aqueous mold release agent which does not impair the mold release property by foaming is obtained.
本発明のＢＮ粉末は、ＢＮ原料を特定のシランカップリング剤で処理することによって製造することができる。本発明で用いられるＢＮ原料には、何ら制約はなく、普通に入手できるもので十分であるが、平均粒子径が１〜２０μｍ、比表面積が２〜５０ｍ２／ｇであるものが好ましい。 The BN powder of the present invention can be produced by treating the BN raw material with a specific silane coupling agent. There are no restrictions on the BN raw material used in the present invention, and those that are usually available are sufficient, but those having an average particle diameter of 1 to 20 μm and a specific surface area of 2 to 50 m 2 / g are preferable.
本発明で使用されるシランカップリング剤は、メトキシ基と、ポリエチレングリコール及びポリプロピレングリコールユニットからなる官能基とを有する分子量２５０以上のシランカップリング剤である。ＢＮは、上記のようにＯＨ基をｃ軸方向にのみ所有しているので、シランカップリング剤により処理される表面積は小さい。そこで、シランカップリング剤の親水効果を更に高めるために、本発明では、メトキシ基と、ポリエチレングリコール及びポリプロピレングリコールユニットからなる官能基とを有するシランカップリング剤を用いる。 The silane coupling agent used in the present invention is a silane coupling agent having a molecular weight of 250 or more having a methoxy group and a functional group composed of polyethylene glycol and polypropylene glycol units. Since BN possesses OH groups only in the c-axis direction as described above, the surface area to be treated with the silane coupling agent is small. Therefore, in order to further enhance the hydrophilic effect of the silane coupling agent, a silane coupling agent having a methoxy group and a functional group composed of polyethylene glycol and polypropylene glycol units is used in the present invention.
しかし、このようにしてシランカップリング剤の親水性を高めただけでは親水効果は必ずしも十分とはならず、シランカップリング剤の付着率の指標である隠蔽性も重要となる。すなわち、ＢＮの粉末度が小さくても大きなカップリング効果を得ることができる隠蔽性の大きなシランカップリング剤であることが好ましい。そこで、分子量が大きく、立体障害の少ない直鎖構造のシランカップリング剤に着目して更に検討したところ、メトキシ基と上記官能基を有する分子量２５０以上のシランカップリング剤が卓越した効果を有することを見いだした。しかも、水分散体の泡立ちが少ない（すなわち消泡性に優れている）作用効果も兼ね備えていたことは全く驚くべきことであり、これによって塗布面には凹凸が生じにくく、作業性の良好な水性の離型剤を得ることができた。 However, simply increasing the hydrophilicity of the silane coupling agent in this way does not necessarily provide a sufficient hydrophilic effect, and concealment, which is an index of the adhesion rate of the silane coupling agent, is also important. That is, it is preferable that the silane coupling agent has a high concealability and can provide a large coupling effect even when the BN fineness is small. Therefore, when further study was made by paying attention to a silane coupling agent having a linear structure having a large molecular weight and little steric hindrance, the silane coupling agent having a methoxy group and the above functional group having a molecular weight of 250 or more has an excellent effect. I found. Moreover, it was quite surprising that the water dispersion also had a low foaming effect (i.e., excellent antifoaming properties), and as a result, the coated surface was less prone to unevenness and good workability. An aqueous release agent could be obtained.
シランカップリング剤の割合は、ＢＮ粉末中、０．５〜１０質量％の含有率である。含有率が０．５質量％よりも著しく小さいと水への十分な分散性が改善されず、また１０質量％よりも著しく大きいとＢＮ粉末がベトついて取り扱いが不便になるばかりでなく、離型剤が過剰のシランカップリング剤によって汚染される。 The ratio of the silane coupling agent is a content of 0.5 to 10% by mass in the BN powder . If the content is significantly smaller than 0.5% by mass, sufficient dispersibility in water cannot be improved. If the content is significantly larger than 10% by mass, the BN powder becomes sticky and inconvenient to handle. The agent is contaminated by excess silane coupling agent.
本発明の離型剤は、本発明の上記ＢＮ粉末を水に分散させた水分散体からなるものである。従来のＢＮ粉末の水分散体の製造には、混合等に長時間を要したが、本発明のＢＮ粉末を使用することで、容易に製造することが可能となり、製造時の作業性が向上する。水分散体中のＢＮ粉末濃度は、１〜３０質量％である。１質量％よりも著しく小さいと離型剤としての性能を十分に発揮せず、また３０質量％よりも著しく大きくなると、塗布・乾燥後の塗膜がひび割れ等を生じる恐れがある。 The release agent of the present invention comprises an aqueous dispersion in which the BN powder of the present invention is dispersed in water. Production of a conventional aqueous dispersion of BN powder took a long time for mixing and the like, but by using the BN powder of the present invention, it can be easily produced and the workability during production is improved. To do. The BN powder concentration in the aqueous dispersion is 1 to 30% by mass . If it is significantly smaller than 1% by mass, the performance as a release agent cannot be sufficiently exhibited, and if it is significantly larger than 30% by mass, the coated / dried coating film may be cracked.
本発明のＢＮ粉末は、ＢＮ原料とシランカップリング剤を混合することによって、また本発明の離型剤は、本発明のＢＮ粉末と水を混合するか、又はＢＮ原料とシランカップリング剤と水を混合することによって、製造することができる。中でも、シランカップリング剤を溶解させた水とＢＮ原料とを混合して離型剤を製造することが好ましい。混合装置としては、サンプルミル、ヘンシェルミキサー、ボールミル、振動ミル、アトライターミル等が使用される。 The BN powder of the present invention is obtained by mixing a BN raw material and a silane coupling agent, and the release agent of the present invention is a mixture of the BN powder of the present invention and water, or a BN raw material and a silane coupling agent. It can be produced by mixing water. Among these, it is preferable to produce a release agent by mixing water in which a silane coupling agent is dissolved and a BN raw material. As a mixing apparatus, a sample mill, a Henschel mixer, a ball mill, a vibration mill, an attritor mill, or the like is used.
参考例１〜３、比較例３、４
市販のＢＮ原料（電気化学工業社製商品名「ＨＧＰ」、平均粒子径５μｍ、比表面積１１ｍ２／ｇ）とシランカップリング剤（信越化学工業社製商品名「Ｘ−１２−６４１Ｓ」、分子量２７０以上）を、表１に示す割合で混合して本発明のＢＮ粉末を製造し、その（１）水中分散性、（２）取扱い性、（３）消泡性を評価した。それらの結果を表１に示す。なお、用いたシランカップリング剤は、メトキシ基と、ポリエチレングリコール及びポリプロピレングリコールユニットからなる官能基とを有するものである。
Reference Examples 1-3, Comparative Examples 3, 4
Commercially available BN raw material (trade name “HGP” manufactured by Denki Kagaku Kogyo Co., Ltd., average particle diameter 5 μm, specific surface area 11 m 2 / g) and silane coupling agent (trade name “X-12-641S” manufactured by Shin-Etsu Chemical Co., Ltd.), molecular weight 270 or more) were mixed at a ratio shown in Table 1 to produce the BN powder of the present invention, and (1) dispersibility in water, (2) handleability, and (3) antifoaming property were evaluated. The results are shown in Table 1. The used silane coupling agent has a methoxy group and a functional group composed of polyethylene glycol and polypropylene glycol units.
比較例１
シランカップリング剤として、３−グリシドキシプロピルトリメトキシシランで構成されるシランカップリング剤（信越化学工業社製商品名「ＫＢＭ−４０３」）を用いたこと以外は、実施例２と同様にしてＢＮ原料を処理した。
Comparative Example 1
Example 2 was used except that a silane coupling agent composed of 3-glycidoxypropyltrimethoxysilane (trade name “KBM-403” manufactured by Shin-Etsu Chemical Co., Ltd.) was used as the silane coupling agent. The BN raw material was processed.
比較例２
シランカップリング剤の代わりに、ポリオキシエチレンソルビタンモノステアレートで構成される界面活性剤（花王社製商品名「レオドールスーパーＴＷ−Ｓ１２０」）を用いたこと以外は、実施例２と同様にしてＢＮ原料を処理した。
Comparative Example 2
Example 2 was used except that a surfactant composed of polyoxyethylene sorbitan monostearate (trade name “Reodol Super TW-S120” manufactured by Kao Corporation) was used instead of the silane coupling agent. The BN raw material was processed.
（１）水中分散性
内径５０〜１００ｍｍの容器に１５０ｍｌの水を加え、撹拌子を用いて４００ｒｐｍで撹拌しながら、ＢＮ粉末０．５ｇを添加し、ＢＮ粉末が水面から見えなくなる速度すなわちＢＮ粉末が水中に完全に分散した時間を測定した。
(1) Dispersibility in water 150 ml of water is added to a container having an inner diameter of 50 to 100 mm, 0.5 g of BN powder is added while stirring at 400 rpm using a stirrer, and the speed at which BN powder becomes invisible from the water surface, that is, BN powder Was measured for the time it was completely dispersed in water.
（２）取扱い性
ＢＮ粉末のベトつき具合を指触により評価した。
○：ベトつきがなく、取り扱い易い
△：ベトつくが、取り扱いづらいほどではない
×：ベトつき、取り扱いづらい
(2) Handleability The stickiness of BN powder was evaluated by finger touch.
○: No stickiness and easy to handle △: Sticky but not so difficult to handle ×: Sticky, difficult to handle
（３）消泡性
水中分散性評価直後の水分散体の水面を観察し、泡立ちが発生している割合を算出した。
○：水面面積に対して泡立ち発生部分の割合が１０％未満
×：水面面積に対して泡立ち発生部分の割合が１０％以上
(3) Antifoaming property The water surface of the water dispersion immediately after the evaluation of dispersibility in water was observed, and the ratio of occurrence of foaming was calculated.
○: The ratio of the foaming portion to the water surface area is less than 10%. X: The ratio of the foaming portion to the water surface area is 10% or more.
実施例６、７
参考例２で得られたＢＮ粉末を用い、そのＢＮ粉末５質量％と純水９５質量％（実施例６）を、又はそのＢＮ粉末２０質量％と純水８０質量％（実施例７）を、ボールミルを用いそれぞれ２時間混合して水性の離型剤を調製した。これを厚み約２０μｍにしてステンレス板に塗布し、１００℃、１時間乾燥させてから、この塗膜上に軟化点約７００℃のガラス（旭製作所製商品名「ルッキングガラス」）を置き、８００℃、１時間加熱した。冷却後にガラスの塗膜からの離型性を評価したところ、いずれも塗膜からガラスを容易に外すことができた。
Examples 6 and 7
Using a BN powder obtained in Reference Example 2, the BN powder 5% by weight and pure water 95 wt% (Example 6), or a BN powder 20 wt% pure water 80% (Example 7) The mixture was mixed for 2 hours using a ball mill to prepare an aqueous release agent. This was applied to a stainless steel plate with a thickness of about 20 μm, dried at 100 ° C. for 1 hour, and then a glass having a softening point of about 700 ° C. (trade name “Looking Glass” manufactured by Asahi Seisakusho) was placed on the coating film. C. for 1 hour. When the releasability from the glass coating film was evaluated after cooling, the glass could be easily removed from the coating film.
本発明のＢＮ粉末は、水性のＢＮ離型剤などのようにＢＮ粉末を水に分散させる用途に使用される。本発明の離型剤は、例えばガラス成型、アルミダイキャスト等の離型剤に使用される。 The BN powder of the present invention is used for applications in which BN powder is dispersed in water, such as an aqueous BN release agent. The mold release agent of the present invention is used for mold release agents such as glass molding and aluminum die casting.
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| JP2004041234A JP4241424B2 (en) | 2004-02-18 | 2004-02-18 | Boron nitride powder and mold release agent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073924A (en) * | 2013-01-23 | 2013-05-01 | 苏州大学 | Boron nitride comprising phosphonitrile structure and preparation method thereof |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7524560B2 (en) * | 2005-08-19 | 2009-04-28 | Momentive Performance Materials Inc. | Enhanced boron nitride composition and compositions made therewith |
| JP4909105B2 (en) * | 2007-02-02 | 2012-04-04 | 電気化学工業株式会社 | Boron nitride containing slurry |
| JP6060060B2 (en) * | 2012-10-11 | 2017-01-11 | 水島合金鉄株式会社 | High oil-absorbing boron nitride powder and cosmetics with excellent heat dissipation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073924A (en) * | 2013-01-23 | 2013-05-01 | 苏州大学 | Boron nitride comprising phosphonitrile structure and preparation method thereof |
| CN103073924B (en) * | 2013-01-23 | 2014-09-17 | 苏州大学 | Boron nitride comprising phosphonitrile structure and preparation method thereof |
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