JP6479167B2 - 超分岐状オレフィン流体を基とする放熱グリス - Google Patents
超分岐状オレフィン流体を基とする放熱グリス Download PDFInfo
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- JP6479167B2 JP6479167B2 JP2017513056A JP2017513056A JP6479167B2 JP 6479167 B2 JP6479167 B2 JP 6479167B2 JP 2017513056 A JP2017513056 A JP 2017513056A JP 2017513056 A JP2017513056 A JP 2017513056A JP 6479167 B2 JP6479167 B2 JP 6479167B2
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- ethylene
- hyperbranched
- olefin
- carbon
- propylene
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- 239000012530 fluid Substances 0.000 title claims description 79
- 239000004519 grease Substances 0.000 title claims description 79
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- 239000005977 Ethylene Substances 0.000 claims description 64
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 63
- 239000000203 mixture Substances 0.000 claims description 63
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 56
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- 239000003054 catalyst Substances 0.000 claims description 52
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 38
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 3
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- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
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- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 3
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- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims 1
- NYMPGSQKHIOWIO-UHFFFAOYSA-N hydroxy(diphenyl)silicon Chemical compound C=1C=CC=CC=1[Si](O)C1=CC=CC=C1 NYMPGSQKHIOWIO-UHFFFAOYSA-N 0.000 claims 1
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Classifications
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Description
(1−F2)/F2=r1(1−f2)/f2 (等式1)
オリゴマー組成物(F)のFTIRまたは13C NMR測定は典型的に、反応性比の決定のために使用され、13C NMRが、好ましい。33〜66%の範囲であるアルファオレフィンモノマー分率(f2)は概して、反応性比の決定のために使用され、50%の値が、好ましい。エチレン−オレフィン反応性比を決定するための好ましい方法は、f1=f2=1/2になるような、アルカンなどの、相溶性のある溶媒中に溶解されたオレフィン及びエチレンの等モルレベルを伴う。低い転換(<20%)へのこの混合物のコオリゴマー化の後、得られたオリゴマー組成物(F)は、反応性比r1を決定するために等式1で使用される。
Tは、好ましい実施形態において、存在する場合、ジアルキルシリル、ジアリールシリル、ジアルキルメチル、エチレニル(−CH2−CH2−)、またはヒドロカルビルエチレニルから選択される任意の架橋基であり、エチレニル中の1個、2個、3個、または4個の水素原子が、ヒドロカルビルにより置換され、ヒドロカルビルが独立して、C1〜C16アルキルまたはフェニル、トリル、キシリルなどであり得る場合、及びTが存在するとき、表される触媒は、ラセミまたはメソの形態にあり得、
L1及びL2は、同じかまたは異なるシクロペンタジエニル、インデニル、テトラヒドロインデニル、またはフルオレニル環であり、任意に置換され、各々Mに結合するか、あるいはL1及びL2は、同じかもしくは異なるシクロペンタジエニル、インデニル、テトラヒドロインデニル、もしくはフルオレニルであり、それらの環は任意に、1つ以上のR基で置換され、任意の2つの隣接するR基は、組み合わさって置換もしくは非置換、飽和、部分的に不飽和、または芳香族環状もしくは多環式置換基を形成し、
Zは、窒素、酸素、またはリンであり、
R’は、環状線状または分岐状C1〜C40アルキルまたは置換アルキル基であり、
X1及びX2は独立して、水素、ハロゲン、水素化ラジカル、ヒドロカルビルラジカル、置換ヒドロカルビルラジカル、ハロカルビルラジカル、置換ハロカルビルラジカル、シリルカルビルラジカル、置換シリルカルビルラジカル、ゲルミルカルビルラジカル、または置換ゲルミルカルビルラジカルであるか、あるいは両方のXは組み合わさり、金属原子に結合して約3〜約20個の炭素原子を含有する金属環状化合物環を形成するか、または両方とも合わせて、オレフィン、ジオレフィン、もしくはアラインリガンドを形成する。
・千個の全炭素当たりのメチン炭素の数
・千個の全炭素当たりのメチル炭素の数
・千個の全炭素当たりのビニル基の数
・千個の全炭素当たりのビニリデン基の数
・千個の全炭素当たりのビニレン基の数
1000/Cn=メチル炭素−メチン炭素−ビニリデン基−ビニレン基(等式2)
1000/Cn=ビニル基+ビニリデン基+ビニレン基(等式3)
1000/Cn=(メチル炭素−メチン炭素+ビニル基)/2(等式4)
Bc=メチン炭素(等式5)
Bn=Bc*Cn/1000(等式6)
Fv=(ビニル基)*Cn/1000(等式7)
Fv=(ビニル基)/(ビニル基+ビニリデン基+ビニレン基)(等式8)
(a)添加されたプロピレンモノマーは、オリゴマー主鎖中に組み込まれたときメチル分岐をもたらすであろう。当業者は、千個の炭素当たりのメチル分岐レベルを算出するために13C NMRスペクトルデータを使用し得る。各メチル分岐は、エチレン及び/またはプロピレン由来でないメチン炭素により伴われることが期待される。よって、エチレン及び/またはプロピレン由来のメチン炭素の分率の算出は、以下に供される。
(b)エチレン由来のメチンの分率=(メチン炭素−メチル分岐)/(メチン炭素)(等式9)
(c)添加されたヘキセンモノマーは、オリゴマー主鎖中に組み込まれたときn−ブチル分岐をもたらすであろう。当業者は、千個の炭素当たりのn−ブチル分岐レベルを算出するために13C NMRスペクトルデータを使用し得る。しかし、いくつかのn−ブチル分岐は、鎖端及びエチレン由来分岐の両方として添加されたヘキセンの不在下で起こることが期待される。それでもなお、全てのn−ブチル分岐の原因を添加されたヘキセンの組み込み結果とすることは、次のようなエチレン由来のメチン炭素の保守的な推定である。
エチレン由来のメチンの分率=(メチン炭素−n−ブチル分岐)/(メチン炭素)(等式10)
千個の炭素当たりの正味の添加されたモノマー=1000*(正味の添加されたモノマーモル)/(オリゴマーとしての炭素の総モル)(等式11)
エチレン由来のメチンの分率=(メチン炭素−千個の炭素当たりの正味の添加されたモノマー)/(メチン炭素)(等式12)
超分岐状オレフィン流体に基づく発明の試料(実施例1a〜1f)の役割を果たす第1のシリーズ、及びシリコーン油に基づく比較試料(比較例1a′〜1f′)の役割を果たす第2のシリーズを用いて、放熱グリス試料を調製する。
好適な超分岐状エチレン系オレフィン流体を調製するために、エチレン、溶媒としてISOPAR−E(商標)、及びトルエン(触媒を溶解するための溶媒として)を含む供給物を活性化アルミナ及びQ−5のカラムに通過させて、第1に水及びそれらからの酸素を除去する。次いで、これらの供給物を、典型的なCSTR逆混合で断熱式の連続攪拌される赤いタンク反応器(CSTR)中に導入し、溶媒(トルエン)、触媒(式V)、及び活性化剤(ISOPAR−E(商標))を、窒素の空気を収容するグローブボックス内に置かれた注射ポンプからステンレス鋼ラインを介して反応器中に導入する。エチレン及び触媒溶液を独立した浸漬管を介して導入し、質量流量制御器を用いて計測する。反応を、60℃の温度で、10分の滞留時間、1.00g/分のC2供給速度、及び0.14のC2モノマーの供給質量分率(C2供給速度/総供給速度)を用いて進める。
マトリックス超分岐状オレフィン流体または選択されたシリコーン油を第1に重量計測し、セラミック円筒カップ中に入れる。グリスの均一性を低減する傾向がある極性問題を克服するために超分岐状流体とのみ使用される界面活性化剤、SPAN(商標)85を重量計測しマトリックス中に添加し、界面活性化剤がマトリックス中に完全混合されるまで、混合物を金属スパチュラで攪拌する。熱伝導性充填剤を重量計測し、激しく手で振動させることにより予備混合する。その後、充填剤をセラミック円筒カップ中に添加し、マトリックスが完全に湿潤した充填剤表面を有していることが視覚的に現れ、複合物が滑らかで、一定のブレンド物として現れるまで金属スパチュラで十分に攪拌及び混練することによりマトリックス混合物中に分散する。攪拌を毎分およそ100旋回(rpm)で3回行い、良好な視覚的均一性を確実にするために、各回少なくとも10分である。得られた放熱グリスを蓋付きのガラスの小瓶中に移動させ、その中で保存する。調製されたグリスは、表4に供される構成成分を有する。
放熱グリスの2つのセットを調製し、第1は、マトリックス構成要素Aとして超分岐状エチレン系及びプロピレン系オレフィン流体を含み、第2は、マトリックス構成要素Aとしてシリコーン流体フェニルメチルポリシロキサンのみを含む。
なお、本発明には、以下の実施態様が包含される。
[1]放熱グリス組成物であって、
(a)超分岐状のエチレン系またはエチレン系及びプロピレン系オレフィン流体であって、1オリゴマー分子当たり平均少なくとも1.5個のメチン炭素を有し、
千個の全炭素当たり少なくとも40個のメチン炭素を有し、
1分子当たりの平均炭素数が、25〜200個である、オレフィン流体と、
(b)熱伝導性充填剤と、の混和物を含む、放熱グリス組成物。
[2]前記超分岐状のエチレン系またはエチレン系及びプロピレン系オレフィン流体が、
(a)ASTM D−93に従って測定されたときに、180℃以上の引火点、
(b)ASTM D−97に従って測定されたときに、ゼロ℃以下の流動点、
(c)ASTM D−445に従って測定されたときに、0.0002平方メートル毎秒以下の40℃での動粘度、及び
(d)これらの組み合わせのうちの少なくとも1つを示す、[1]に記載の放熱グリス組成物。
[3]前記エチレン系またはエチレン系及びプロピレン系流体が、プロピレン以外のアルファ−オレフィンコモノマーをさらに含む、[1]に記載の放熱グリス組成物。
[4]前記熱伝導性充填剤が、酸化ベリリウム、窒化アルミニウム、窒化ホウ素、酸化アルミニウム、酸化亜鉛、酸化マグネシウム、炭化ケイ素、窒化ケイ素、二酸化ケイ素、及び硫化亜鉛;銀、銅、及びアルミニウムから選択される固体金属粒子;ダイヤモンド粉末から選択される炭素材料;炭素繊維、炭素ナノチューブ、カーボンブラック、黒鉛、グラフェン、及び酸化グラフェン;ガリウム系合金から選択される液体金属;ならびにこれらの組み合わせから選択される、[1]に記載の放熱グリス組成物。
[5]相間離隔剤、界面活性化剤、難燃剤、抗酸化剤、結合剤、ブリード阻害剤、レオロジー改質剤、充填剤、またはこれらの組み合わせをさらに含む、[1]に記載の放熱グリス組成物。
[6]前記相間離隔剤が、ポリジメチルシロキサン;フェニルメチルポリシロキサン;ヒドロキシ末端ポリジメチル−シロキサン;ポリジメチルジフェニルシロキサン;ポリジフェニルシロキサン;ナフチル基、エチル基、プロピル基、またはアミル基から選択されるアルキル基を含有するメチルアルキルポリシロキサン;及びこれらの組み合わせから選択される化合物である、[5]に記載の放熱グリス組成物。
[7]放熱グリス組成物を調製するための方法であって、
(a)エチレン、及び任意にプロピレン、及びさらに任意にアルファ−オレフィンと、少なくとも1つの配位挿入触媒とを、少なくとも2つの生成物の混合物が形成されるような条件下で、連続供給逆混合反応器領域内で共に接触させることであって、
前記配位挿入触媒が、金属−リガンド錯体であり、前記金属が、ジルコニウム、ハフニウム、及びチタンから選択され、
かつ最大20のエチレン/オクテン反応性比、及び最大20モノマー単位の動力学的鎖長を有し、
前記混合物が、
(i)超分岐状オリゴマーであって、
1オリゴマー分子当たり平均少なくとも1.5個のメチン炭素を有し、
千個の全炭素当たり少なくとも40個のメチン炭素を有し、
前記メチン炭素の少なくとも40パーセントが、前記エチレン、または前記任意のプロピレンが含まれる場合、前記エチレン及び前記プロピレン由来であり、
1分子当たりの平均炭素数が、25〜200個である、超分岐状オリゴマーと、
(ii)14以下である1分子当たりの平均炭素数を有する少なくとも1つの有機揮発生成物と、を含む、接触させることと、
(b)前記有機揮発生成物から前記超分岐状オリゴマーを分離することと、
(c)前記超分岐状オリゴマーを回収することと、
(d)前記超分岐状オリゴマー及び熱伝導性充填剤を混和して、
放熱グリス組成物を形成することと、を含む、方法。
Claims (7)
- 放熱グリス組成物であって、
(a)超分岐状のエチレン系またはエチレン系及びプロピレン系オレフィン流体であって、1オリゴマー分子当たり平均少なくとも1.5個のメチン炭素を有し、
千個の全炭素当たり少なくとも40個のメチン炭素を有し、
1分子当たりの平均炭素数が、25〜200個である、オレフィン流体20体積%〜40体積%と、
(b)熱伝導性充填剤60体積%〜80体積%と、の混和物を含み、
前記伝導性充填剤が、前記オレフィン流体に中に分散されている、放熱グリス組成物。 - 前記超分岐状のエチレン系またはエチレン系及びプロピレン系オレフィン流体が、
(a)ASTM D−93に従って測定されたときに、180℃以上の引火点、
(b)ASTM D−97に従って測定されたときに、ゼロ℃以下の流動点、及び
(c)ASTM D−445に従って測定されたときに、0.0002平方メートル毎秒以下の40℃での動粘度を示す、請求項1に記載の放熱グリス組成物。 - 前記エチレン系またはエチレン系及びプロピレン系流体が、プロピレン以外のアルファ−オレフィンコモノマーをさらに含む、請求項1に記載の放熱グリス組成物。
- 前記熱伝導性充填剤が、酸化ベリリウム、窒化アルミニウム、窒化ホウ素、酸化アルミニウム、酸化亜鉛、酸化マグネシウム、炭化ケイ素、窒化ケイ素、二酸化ケイ素、及び硫化亜鉛;銀、銅、及びアルミニウムから選択される固体金属粒子;ダイヤモンド粉末から選択される炭素材料;炭素繊維、炭素ナノチューブ、カーボンブラック、黒鉛、グラフェン、及び酸化グラフェン;ガリウム系合金から選択される液体金属;ならびにこれらの組み合わせから選択される、請求項1に記載の放熱グリス組成物。
- 相間離隔剤、界面活性化剤、難燃剤、抗酸化剤、結合剤、ブリード阻害剤、レオロジー改質剤、充填剤、またはこれらの組み合わせをさらに含む、請求項1に記載の放熱グリス組成物。
- 前記相間離隔剤が、ポリジメチルシロキサン;フェニルメチルポリシロキサン;ヒドロキシ末端ポリジメチル−シロキサン;ポリジメチルジフェニルシロキサン;ポリジフェニルシロキサン;ナフチル基、エチル基、プロピル基、またはアミル基から選択されるアルキル基を含有するメチルアルキルポリシロキサン;及びこれらの組み合わせから選択される化合物である、請求項5に記載の放熱グリス組成物。
- 放熱グリス組成物を調製するための方法であって、
(a)エチレン、及び任意にプロピレン、及びさらに任意にアルファ−オレフィンと、少なくとも1つの配位挿入触媒とを、少なくとも2つの生成物の混合物が形成されるような条件下で、連続供給逆混合反応器領域内で共に接触させることであって、
前記配位挿入触媒が、式Vで示される化合物及び式Xで示される化合物:
から選択され、
かつ最大20のエチレン/オクテン反応性比、及び最大20モノマー単位の動力学的鎖長を有し、
前記混合物が、
(i)超分岐状オリゴマーであって、
1オリゴマー分子当たり平均少なくとも1.5個のメチン炭素を有し、
千個の全炭素当たり少なくとも40個のメチン炭素を有し、
前記メチン炭素の少なくとも40パーセントが、前記エチレン、または前記任意のプロピレンが含まれる場合、前記エチレン及び前記プロピレン由来であり、
1分子当たりの平均炭素数が、25〜200個である、超分岐状オリゴマーと、
(ii)14以下である1分子当たりの平均炭素数を有する少なくとも1つの有機揮発生成物と、を含む、接触させることと、
(b)前記有機揮発生成物から前記超分岐状オリゴマーを分離することと、
(c)前記超分岐状オリゴマーを回収することと、
(d)前記超分岐状オリゴマー及び熱伝導性充填剤を混和して、
放熱グリス組成物を形成することと、を含む、方法。
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