JP2011068757A - Magnesium oxide-based highly water-resistant thermoconductive filler, method for producing the same, and resin composition - Google Patents
Magnesium oxide-based highly water-resistant thermoconductive filler, method for producing the same, and resin composition Download PDFInfo
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Abstract
Description
本発明は、合成樹脂に配合する酸化マグネシウムフィラーの製造方法及び樹脂組成物に関する。さらに詳しくは、熱伝導性、耐水性、加工性に優れた樹脂組成物を提供するものである。 The present invention relates to a method for producing a magnesium oxide filler to be blended with a synthetic resin and a resin composition. More specifically, the present invention provides a resin composition excellent in thermal conductivity, water resistance, and processability.
従来より、酸化マグネシウムは高い熱伝導性を有するフィラーとして、樹脂組成物に配合されてきた。しかし、酸化マグネシウム固有の特性である低耐水性が問題となり、耐水性を改善する検討も多数行われてきた。
特許文献１と特許文献２では、ＭｇＯ粉末表面をリン酸マグネシウム系化合物による被覆層を形成し、被覆酸化マグネシウム粉末に対してさらにエチルシリケートを被覆して耐水性を改善している。
特許文献３では、ケイ素とマグネシウムとの複酸化物により、マグネシア粉末の表面を被覆して耐水和性（耐湿性）を改善している。
特許文献４と特許文献５では、アルミニウムとマグネシウムとの複酸化物により、マグネシア粉末の表面を被覆して耐水和性（耐湿性）を改善している。
特許文献６では、酸性リン酸エステルで表面処理して、高耐水和性を改善している。
特許文献７では、死焼マグネシアをカップリング剤で表面処理し、２５０〜８５０℃で再焼成して耐水性を改善している。
特許文献８では、酸化マグネシウムの表面に有機シラン層を形成させて高耐水和性に改善している。
特許文献９では、酸化マグネシウムの表面にシリコーンオイルを焼き付けることにより、耐水性を改善している。
特許文献１０では、マグネシア粉末に有機珪素化合物を添加した後、加熱処理して、耐水性を改善している。
特許文献１１では、シリコーンオイル、シランカップリング剤で酸化マグネシウムを表面処理し、加熱処理して耐水性を改善している。
特許文献１２では、ガラス成分（ＰｂＯを５０wt％以上含有し、残りの成分がＢ2 Ｏ3 ，ＳｉＯ2 のうち少なくとも１種類以上である成分組成であることを特徴とするガラス）を被覆して耐水性を改善している。
Conventionally, magnesium oxide has been blended in resin compositions as a filler having high thermal conductivity. However, low water resistance, which is a characteristic unique to magnesium oxide, has become a problem, and many studies have been conducted to improve water resistance.
In Patent Document 1 and Patent Document 2, a coating layer made of a magnesium phosphate compound is formed on the MgO powder surface, and the coated magnesium oxide powder is further coated with ethyl silicate to improve water resistance.
In Patent Document 3, the surface of magnesia powder is coated with a double oxide of silicon and magnesium to improve hydration resistance (moisture resistance).
In Patent Document 4 and Patent Document 5, the surface of magnesia powder is coated with a double oxide of aluminum and magnesium to improve hydration resistance (humidity resistance).
In Patent Document 6, surface treatment is performed with an acidic phosphate to improve high hydration resistance.
In patent document 7, dead-burned magnesia is surface-treated with a coupling agent and refired at 250 to 850 ° C. to improve water resistance.
In Patent Document 8, an organic silane layer is formed on the surface of magnesium oxide to improve high hydration resistance.
In Patent Document 9, water resistance is improved by baking silicone oil on the surface of magnesium oxide.
In Patent Document 10, after adding an organosilicon compound to magnesia powder, heat treatment is performed to improve water resistance.
In Patent Literature 11, magnesium oxide is surface-treated with silicone oil and a silane coupling agent, and heat resistance is improved by heat treatment.
In Patent Document 12, the glass component (glass characterized by containing 50 wt% or more of PbO and the remaining component having at least one component selected from B2 O3 and SiO2) is coated with water resistance. It has improved.
上記のように、酸化マグネシウムの耐水性を改善すべく、酸化マグネシウムの表面をケイ酸やリン酸で被覆する方法、シリコーンオイルやシランカップリング剤等で被覆、ガラス成分で被覆する方法が検討されてきた。しかし、これら従来の方法ではある程度の耐水性を付与することはできるが充分ではなく、生産性やコスト面の問題も解決されていなかった。 As described above, in order to improve the water resistance of magnesium oxide, a method of coating the surface of magnesium oxide with silicic acid or phosphoric acid, a method of coating with silicone oil or a silane coupling agent, or a method of coating with a glass component has been studied. I came. However, these conventional methods can provide a certain level of water resistance, but are not sufficient, and the problems of productivity and cost have not been solved.
本発明者は、ＢＥＴ比表面積が０．１〜１００ｍ2/ｇ、平均２次粒子径が０．５〜２０μｍの酸化マグネシウムを式（１）に記載のアルキルアルコキシシランで表面被覆することにより、熱伝導性、耐水性、生産性をバランス良く付与でき、コスト面の問題も解決できることを見出し、本発明を完成するに至った。
(CkH(2k+1))n-Si-(OCmH(2m+1))(4-n) [k：６以上、m：２以下、n：１〜３] 式（１）
The inventors have surface-coated magnesium oxide having a BET specific surface area of 0.1 to 100 m 2 / g and an average secondary particle size of 0.5 to 20 μm with the alkylalkoxysilane described in the formula (1), The present inventors have found that heat conductivity, water resistance, and productivity can be imparted in a well-balanced manner and that cost problems can be solved, and the present invention has been completed.
(C k H (2k + 1) ) n -Si- (OC m H (2m + 1) ) (4-n) [k: 6 or more, m: 2 or less, n: 1 to 3] Formula (1)
本発明の酸化マグネシウム系フィラーは、ＢＥＴ比表面積と平均２次粒子径が所定の範囲であれば、軽焼マグネシア、硬焼マグネシア、電融マグネシアのいずれの形態でも対応できる。 As long as the BET specific surface area and the average secondary particle diameter are in a predetermined range, the magnesium oxide filler of the present invention can be used in any form of light-burned magnesia, hard-burned magnesia, and electrofused magnesia.
酸化マグネシウムのＢＥＴ比表面積は０．１〜１００ｍ2/ｇ、平均２次粒子径は０．５〜２０μｍであり、樹脂への充填性やハンドリング性の観点からＢＥＴ比表面積は１〜２０ｍ2/ｇの範囲がより好ましい。 Magnesium oxide has a BET specific surface area of 0.1 to 100 m 2 / g and an average secondary particle size of 0.5 to 20 μm. From the viewpoint of resin filling and handling properties, the BET specific surface area is 1 to 20 m 2 / g. The range of g is more preferable.
平均２次粒子径は、レーザー回折法粒度分布計を用いて測定した値である。測定はエタノール中に測定許容濃度になるように粉末を懸濁させ、超音波分散機等で分散させてから行う。 The average secondary particle diameter is a value measured using a laser diffraction particle size distribution analyzer. The measurement is carried out after suspending the powder in ethanol so as to obtain a measurement allowable concentration and dispersing it with an ultrasonic disperser or the like.
本発明の酸化マグネシウム系フィラーは、１〜１０質量％の(CkH(2k+1))n-Si-(OCmH(2m+1))(4-n) [k：６以上、m：２以下、n：１〜３]で表面被覆して調製される。被覆量が１質量％より少ないと、未被覆部分が残るため耐水性が不十分となる。また、被覆量が１０質量％を越えると、コストアップにつながり、好ましくない。
なお、乾式処理に用いる装置は、例えばヘンシェルミキサー等の高速攪拌混合可能なものが効率的に被覆処理できるため好ましい。
The magnesium oxide filler of the present invention is 1 to 10% by mass of (C k H (2k + 1) ) n —Si— (OC m H (2m + 1) ) (4-n) [k: 6 or more, m: 2 or less, n: 1 to 3]. If the coating amount is less than 1% by mass, the uncoated portion remains, resulting in insufficient water resistance. On the other hand, if the coating amount exceeds 10% by mass, the cost increases, which is not preferable.
In addition, as the apparatus used for the dry treatment, for example, a device capable of high-speed stirring and mixing such as a Henschel mixer can be efficiently coated.
本発明で用いる被覆剤は、(CkH(2k+1))n-Si-(OCmH(2m+1))(4-n) [k：６以上、m：２以下、n：１〜３]である。デシルトリメトキシシラン、オクチルトリメトキシシラン、ヘキシルトリメトキシシラン、ヘキシルトリエトキシシラン等が使用でき、極性が小さいので通常のシランカップリング剤やシリコーンオイルに較べて撥水性が高く、高い耐水性が付与されるものと考えられる。 The coating agent used in the present invention is (C k H (2k + 1) ) n -Si- (OC m H (2m + 1) ) (4-n) [k: 6 or more, m: 2 or less, n: 1-3]. Decyltrimethoxysilane, octyltrimethoxysilane, hexyltrimethoxysilane, hexyltriethoxysilane, etc. can be used, and since it has low polarity, it has higher water repellency compared to ordinary silane coupling agents and silicone oils, giving it high water resistance It is considered to be done.
本発明の樹脂組成物は、表面被覆された上記の酸化マグネシウム系フィラーを１００質量部の合成樹脂に対して１００〜５００質量部配合したものである。使用する合成樹脂は、ポリアミド、ポリアセタール、ポリブチレンテレフタレート、ポリエチレンテレフタレート、シンジオタクチックポリスチレン、ポリフェニレンサルファイド、液晶ポリマー、ポリエーテルケトン、ポリエーテルニトリル、ポリカーボネート、変性ポリフェニレンエーテル、ポリサルホン、ポリエーテルサルホン、ポリアリレート、ポリアミドイミド、ポリエーテルイミド、熱可塑性ポリイミド等が挙げられる。 The resin composition of this invention mix | blends 100-500 mass parts of said magnesium oxide type fillers by which surface coating was carried out with respect to 100 mass parts synthetic resin. Synthetic resins used are polyamide, polyacetal, polybutylene terephthalate, polyethylene terephthalate, syndiotactic polystyrene, polyphenylene sulfide, liquid crystal polymer, polyether ketone, polyether nitrile, polycarbonate, modified polyphenylene ether, polysulfone, polyether sulfone, poly Examples include arylate, polyamideimide, polyetherimide, and thermoplastic polyimide.
本発明の樹脂組成物は、例えば自動車分野の排ガスバルブ、ランプソケット、各種電装部品、ＯＡ・ＡＶ機器分野のビデオＣＤ・ＤＶＤピックアップ部品、各種コネクター、スイッチ、軸受け、ケースハウジングなどがあげられる。さらに表面実装電子部材(ＩＣ部品などの封止)にも適用できる。 Examples of the resin composition of the present invention include exhaust gas bulbs, lamp sockets, various electrical components in the automotive field, video CD / DVD pickup components in the OA / AV equipment field, various connectors, switches, bearings, case housings, and the like. Further, it can be applied to surface mount electronic members (sealing of IC components and the like).
本発明では、熱伝導性、耐水性、生産性、コストのバランスのとれた合成樹脂配合用の酸化マグネシウム系高耐水性熱伝導フィラー及びその製造方法、樹脂組成物を提供する。 The present invention provides a magnesium oxide-based highly water-resistant heat conductive filler for synthetic resin blending, which has a good balance of thermal conductivity, water resistance, productivity, and cost, a method for producing the same, and a resin composition.
以下に本発明の実施例を示す。 Examples of the present invention are shown below.
フィラーの調製
基材となる酸化マグネシウムの調製方法および性状を表１に示す。
Table 1 shows the preparation method and properties of magnesium oxide used as the filler preparation base material.
実施例１
酸化マグネシウム（Ａ）５００ｇをヘンシェルミキサー(三井三池化工製、容量３０Ｌ)に入れ、攪拌しながらデシルトリメトキシシラン１０ｇを徐々に添加した。添加終了後、１５０℃で３０分間表面被覆処理を行い、酸化マグネシウム系フィラー（Ａ-1）を得た。
Example 1
Magnesium oxide (A) (500 g) was placed in a Henschel mixer (manufactured by Mitsui Miike Chemical Co., Ltd., capacity: 30 L), and 10 g of decyltrimethoxysilane was gradually added while stirring. After completion of the addition, a surface coating treatment was performed at 150 ° C. for 30 minutes to obtain a magnesium oxide filler (A-1).
実施例２〜実施例３
表１に示す酸化マグネシウム（Ｂ、Ｃ）を使用した以外は、実施例1と同様にして、酸化マグネシウム系フィラー（Ｂ-１、Ｃ-１）を得た。
Example 2 to Example 3
Magnesium oxide fillers (B-1, C-1) were obtained in the same manner as in Example 1 except that the magnesium oxides (B, C) shown in Table 1 were used.
実施例４
実施例１の被覆剤を２５ｇのヘキシルトリメトキシシランに変えた以外は同様に行って、酸化マグネシウム系フィラー（Ａ-２）を得た。
Example 4
A magnesium oxide filler (A-2) was obtained in the same manner except that the coating agent of Example 1 was changed to 25 g of hexyltrimethoxysilane.
比較例１
表１の酸化マグネシウム（Ａ）を被覆剤で処理せずに酸化マグネシウム系フィラー（Ａ-３）とした。
Comparative Example 1
Magnesium oxide (A) in Table 1 was not treated with a coating agent, and was used as a magnesium oxide filler (A-3).
比較例２
実施例１の被覆剤をジメチルジメトキシシランに変えた以外は同様に行って、酸化マグネシウム系フィラー（Ａ-４）を得た。
Comparative Example 2
A magnesium oxide filler (A-4) was obtained in the same manner except that the coating agent of Example 1 was changed to dimethyldimethoxysilane.
比較例３
実施例１の被覆剤をジフェニルジメトキシシランに変えた以外は同様に行って、酸化マグネシウム系フィラー（Ａ-５）を得た。
Comparative Example 3
A magnesium oxide filler (A-5) was obtained in the same manner except that the coating agent of Example 1 was changed to diphenyldimethoxysilane.
比較例４
実施例１の被覆剤をエポキシシランカップリング剤に変えた以外は同様に行って、酸化マグネシウム系フィラー（Ａ-６）を得た。
Comparative Example 4
A magnesium oxide filler (A-6) was obtained in the same manner except that the coating agent of Example 1 was changed to an epoxy silane coupling agent.
比較例５
実施例１の被覆剤をリン酸エステルに変えた以外は同様に行って、酸化マグネシウム系フィラー（Ａ-７）を得た。
Comparative Example 5
A magnesium oxide filler (A-7) was obtained in the same manner except that the coating agent of Example 1 was changed to a phosphate ester.
比較例６
実施例１の被覆剤の処理量を２.５ｇに変えた以外は同様に行って、酸化マグネシウム系フィラー（Ａ-８）を得た。
Comparative Example 6
A magnesium oxide filler (A-8) was obtained in the same manner except that the treatment amount of the coating agent of Example 1 was changed to 2.5 g.
比較例７
酸化マグネシウム（Ａ）５００gをヘンシェルミキサー(三井三池化工製、容量３０Ｌ)に入れ、撹拌しながらアルコキシ変性シリコンオイル１０ｇを徐々に添加した。添加終了後、ステンレス製トレーに移し、送風乾燥機中で、３００℃、１時間加熱処理して、酸化マグネシウム系フィラー（Ａ-９）を得た。
Comparative Example 7
Magnesium oxide (A) (500 g) was put into a Henschel mixer (manufactured by Mitsui Miike Chemical Co., Ltd., volume 30 L), and 10 g of alkoxy-modified silicone oil was gradually added while stirring. After completion of the addition, the mixture was transferred to a stainless steel tray and subjected to heat treatment at 300 ° C. for 1 hour in a blast dryer to obtain a magnesium oxide filler (A-9).
比較例８
酸化マグネシウム（Ａ）５００gとデシルトリメトキシシラン１０ｇをエタノール５Ｌに分散させ、１時間混合撹拌後、ろ過、乾燥、解砕して、酸化マグネシウム系フィラー（Ａ-１０）を得た。
Comparative Example 8
Magnesium oxide (A) 500 g and decyltrimethoxysilane 10 g were dispersed in 5 L of ethanol, mixed and stirred for 1 hour, filtered, dried and crushed to obtain a magnesium oxide filler (A-10).
比較例９
酸化マグネシウム（Ｄ）５００gとヒュームドシリカ５０ｇをエタノール５Ｌに分散させ、１０分間撹拌混合した。ろ過、乾燥した後、衝撃型粉砕機で解砕し、１４００℃で１時間加熱処理し、酸化マグネシウム系フィラー（Ｄ-１）を得た。
Comparative Example 9
Magnesium oxide (D) (500 g) and fumed silica (50 g) were dispersed in ethanol (5 L) and mixed with stirring for 10 minutes. After filtration and drying, the mixture was pulverized with an impact pulverizer and heat-treated at 1400 ° C. for 1 hour to obtain a magnesium oxide filler (D-1).
実施例１〜４及び比較例１〜９で得られた酸化マグネシウム系フィラーについて耐水性試験を行った。
「耐水性試験」：秤量瓶に試料２．０ｇを入れ、温度８５℃/湿度８５％の恒温恒湿槽中に１週間放置後、試験前後の重量変化を測定した。
重量変化が１.０重量％未満であれば良好とし、１.０重量％以上を不良とした。試験結果を表２に示す。
A water resistance test was performed on the magnesium oxide fillers obtained in Examples 1 to 4 and Comparative Examples 1 to 9.
“Water resistance test”: 2.0 g of a sample was placed in a weighing bottle and left in a constant temperature and humidity chamber at a temperature of 85 ° C./humidity of 85% for 1 week, and the weight change before and after the test was measured.
A weight change of less than 1.0% by weight was considered good, and 1.0% by weight or more was judged bad. The test results are shown in Table 2.
表２の実施例１〜４の結果より、本発明の請求項で規定したＢＥＴ比表面積と平均２次粒子径を有する酸化マグネシウムを所定の被覆剤で処理することにより耐水性の良好な酸化マグネシウムが得られることがわかる。
しかし、比較例６のように本発明の請求項で規定した酸化マグネシウムを所定の被覆剤で処理しても、被覆剤量が所定量以下であると耐水性は改善されない。
また、比較例２〜５及び比較例７〜８のように、従来検討されてきた被覆剤を同様に処理しても、耐水性は本発明の実施例と比較していずれも劣り、不良の評価であった。
なお、比較例９の耐水性評価は良好の範囲であったが、本発明の実施例に較べると劣っていた。
From the results of Examples 1 to 4 in Table 2, magnesium oxide having good water resistance can be obtained by treating magnesium oxide having a BET specific surface area and an average secondary particle diameter defined in the claims of the present invention with a predetermined coating agent. It can be seen that
However, even if the magnesium oxide specified in the claims of the present invention is treated with a predetermined coating agent as in Comparative Example 6, the water resistance is not improved if the coating amount is not more than the predetermined amount.
In addition, as in Comparative Examples 2 to 5 and Comparative Examples 7 to 8, even if the conventionally studied coating agents are treated in the same manner, the water resistance is inferior to that of the Examples of the present invention and is poor. It was evaluation.
In addition, although the water resistance evaluation of the comparative example 9 was the favorable range, it was inferior compared with the Example of this invention.
樹脂組成物の調製Preparation of resin composition
実施例１１
ポリアミド樹脂１００質量部に対し、酸化マグネシウム系フィラー（Ａ-１）３００質量部を配合して、２５０℃で５分間混練した。混練物を金型（１５０×５０×１０ｍｍ）に入れ、２０ＭＰａに加圧して２５０℃で５分間プレスして成型体を作製した。
Example 11
300 parts by mass of magnesium oxide filler (A-1) was blended with 100 parts by mass of the polyamide resin, and kneaded at 250 ° C. for 5 minutes. The kneaded product was put into a mold (150 × 50 × 10 mm), pressurized to 20 MPa and pressed at 250 ° C. for 5 minutes to prepare a molded body.
実施例１２〜１４及び比較例１１〜１９
実施例２〜４及び比較例１〜９で得られた酸化マグネシウム系フィラー（Ｂ-１、Ｃ-１、Ａ-２、Ａ-３、Ａ-４、Ａ-５、Ａ-６、Ａ-７、Ａ-８、Ａ-９、Ａ-１０、Ｄ-１）について、実施例１１と同様にして成型体を得た。
Examples 12-14 and Comparative Examples 11-19
Magnesium oxide fillers obtained in Examples 2 to 4 and Comparative Examples 1 to 9 (B-1, C-1, A-2, A-3, A-4, A-5, A-6, A- 7, A-8, A-9, A-10, D-1) were obtained in the same manner as in Example 11 to obtain a molded product.
上記の方法により作製した樹脂組成物成型体の熱伝導率を測定した。
「熱伝導率測定」：ＡＳＴＭ−Ｅ１５０３に準拠して測定した。熱伝導率が３．０Ｗ/ｍＫ以上であれば良好とし、それより小さいものは不良とした。測定結果を表３に示す。
The thermal conductivity of the molded resin composition produced by the above method was measured.
“Thermal conductivity measurement”: Measured according to ASTM-E1503. A thermal conductivity of 3.0 W / mK or higher was considered good, and a smaller thermal conductivity was considered defective. Table 3 shows the measurement results.
表３の結果より、実施例１１〜１４と比較例１１を較べると明らかに実施例の熱伝導率が良好であることがわかる。これは、本発明の請求項に規定の酸化マグネシウムであっても被覆剤で処理されていないため、樹脂組成物の混練時に酸化マグネシウムが樹脂中に均一に分散しなかったためと推察する。
また、比較例１４は処理剤にエポキシシランカップリング剤を用いたもので、比較的良好な熱伝導率を示したが、耐水性評価が不良であり使用できない。
耐水性が良好で樹脂に混練した時の樹脂組成物の熱伝導率が良好な酸化マグネシウムは、本発明の請求項に記載のＢＥＴ比表面積と平均２次粒子径を有する酸化マグネシウムを本発明の請求項に記載の被覆剤で処理した酸化マグネシウム系フィラーである。
From the results of Table 3, it can be seen that when Examples 11 to 14 and Comparative Example 11 are compared, the thermal conductivity of Examples is clearly good. This is presumably because the magnesium oxide specified in the claims of the present invention was not treated with the coating agent, so that the magnesium oxide was not uniformly dispersed in the resin during the kneading of the resin composition.
Moreover, although the comparative example 14 used the epoxy silane coupling agent for the processing agent and showed comparatively favorable heat conductivity, water resistance evaluation is unsatisfactory and cannot be used.
Magnesium oxide having good water resistance and good thermal conductivity of the resin composition when kneaded with resin is magnesium oxide having a BET specific surface area and an average secondary particle diameter according to the claims of the present invention. A magnesium oxide filler treated with the coating agent according to claim.
Claims (4)
(CkH(2k+1))n-Si-(OCmH(2m+1))(4-n) [k：6以上、m：2以下、n：1〜3] 式（１） Magnesium oxide having a BET specific surface area of 0.1 to 100 m 2 / g and an average secondary particle diameter of 0.5 to 20 μm, which is obtained by coating the coating agent of formula (1) with 1 to 10% by mass with respect to magnesium oxide. A highly water resistant heat conductive filler characterized by being.
(C k H (2k + 1) ) n -Si- (OC m H (2m + 1) ) (4-n) [k: 6 or more, m: 2 or less, n: 1 to 3] Formula (1)
The resin composition which mix | blended 100-500 mass parts of the highly water-resistant heat conductive fillers of Claim 1 or Claim 2 with respect to 100 mass parts of synthetic resins.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2014119462A1 (en) * | 2013-01-30 | 2014-08-07 | Dic株式会社 | Heat-conductive filler, method for producing said filler, resin composition using said filler, molded article produced from said resin composition, and highly heat-conductive material |
| WO2018180123A1 (en) * | 2017-03-28 | 2018-10-04 | 宇部マテリアルズ株式会社 | Coated magnesium oxide particle and method for producing same, and thermally conductive resin composition |
| US10121717B2 (en) | 2014-09-29 | 2018-11-06 | Sekisui Chemical Co., Ltd. | Carbon-coated thermal conductive material |
| WO2021193690A1 (en) * | 2020-03-26 | 2021-09-30 | 日本アエロジル株式会社 | Insulating filler and production method therefor, insulating material containing said insulating filler and production method therefor |
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| US11718729B2 (en) | 2020-03-26 | 2023-08-08 | Nippon Aerosil Co., Ltd. | Insulating filler and production method therefor, insulating material containing said insulating filler and production method therefor |
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