JPWO2019203210A1 - 潤滑油組成物および潤滑油用粘度調整剤 - Google Patents
潤滑油組成物および潤滑油用粘度調整剤 Download PDFInfo
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- JPWO2019203210A1 JPWO2019203210A1 JP2020514385A JP2020514385A JPWO2019203210A1 JP WO2019203210 A1 JPWO2019203210 A1 JP WO2019203210A1 JP 2020514385 A JP2020514385 A JP 2020514385A JP 2020514385 A JP2020514385 A JP 2020514385A JP WO2019203210 A1 JPWO2019203210 A1 JP WO2019203210A1
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- Prior art keywords
- lubricating oil
- copolymer
- viscosity
- ethylene
- oil composition
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Classifications
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
- C10M143/08—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation containing aliphatic monomer having more than 4 carbon atoms
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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Abstract
Description
本発明の潤滑油組成物は、特定のエチレン・α−オレフィン共重合体(A)を含有し、好ましくはさらに潤滑油基油(B)を含有する。ここで、共重合体(A)は、潤滑油用粘度調整剤として機能することができる。
本発明で使用されるエチレン・α−オレフィン共重合体(A)(以下「共重合体(A)」ともいう)について説明する。共重合体(A)は、エチレン由来の構成単位の含有割合が70〜90モル%であり、極限粘度[η]が0.3〜1.0dl/gである。
本発明の潤滑油組成物、例えばエンジン用潤滑油組成物は、潤滑油基油(B)(以下「基油(B)」ともいう)をさらに含有することが好ましい。基油(B)は、通常、エンジン用潤滑油基油などの潤滑油基油として用いられるものを制限なく用いることができ、例えば、鉱物油、合成油が挙げられる。基油(B)としては、鉱物油と合成油とのブレンド物を用いてもよい。
*2:ASTM D3238に準じて測定
*3:ASTM D4294(JIS K2541)に準じて測定
*4:飽和炭化水素分が90(vol%)未満でかつ硫黄分が0.03質量%未満または飽和炭化水素分が90(vol%)以上でかつ硫黄分が0.03質量%を超える鉱物油もグループ(I)に含まれる。
本発明の潤滑油組成物、例えばエンジン用潤滑油組成物は、共重合体(A)および基油(B)以外の他の成分(添加剤)を含有することができる。他の成分としては、例えば、共重合体(A)以外の他の粘度調整剤、流動点降下剤、清浄分散剤、摩耗防止剤、消泡剤、酸化防止剤、摩擦調整剤、色安定剤、錆止め剤、腐食防止剤および金属不活性化剤が挙げられる。
本発明の潤滑油組成物、例えばエンジン用潤滑油組成物は、従来公知の方法で、例えば共重合体(A)、必要に応じて基油(B)および添加剤を混合することにより調製することができる。共重合体(A)は、取扱いが容易なため、基油(B)中の濃縮物として任意に供給してもよい。
本発明の潤滑油組成物は、例えば高温でのエンジン作動中の燃費性を改善するため、高温低剪断速度下での粘度が低いことが好ましい。すなわち、本発明の潤滑油組成物は、100℃における動粘度が、通常は50mm2/s以下であり、好ましくは1〜40mm2/s、より好ましくは2〜30mm2/sである。
本発明の潤滑油用粘度調整剤は、前述した第1の態様の、エチレンと炭素数4以上のα−オレフィンとの共重合体(A)を含有する。第1の態様の共重合体(A)の好ましい要件は、前述したとおりである。
本発明のエンジン用潤滑油のための粘度調整剤は、前述した第2の態様のエチレン・α−オレフィン共重合体(A)を含有する。ここで、前記共重合体(A)におけるエチレン由来の構成単位の含有割合は、79〜90mol%である。共重合体(A)のその他の好ましい要件は、前述したとおりである。
共重合体の各種物性は、以下のようにして測定した。
共重合体の極限粘度[η]は、デカリン溶媒を用いて、135℃で測定した。具体的には、共重合体のパウダー、ペレットまたは樹脂塊約20mgをデカリン15mlに溶解し、135℃のオイルバス中で比粘度ηspを測定した。このデカリン溶液にデカリン溶媒を5ml追加して希釈後、同様にして比粘度ηspを測定した。この希釈操作をさらに2回繰り返し、濃度(C)を0に外挿した時のηsp/Cの値を極限粘度として求めた(下式参照)。
<エチレン単位の含有割合(C2含量)>
エチレン・α−オレフィン共重合体におけるエチレン由来の構成単位の含有割合およびα−オレフィン由来の構成単位の含有割合(モル%)については、13C−NMRスペクトルの解析により求めた。
ブルカーバイオスピン社製AVANCEIII500CryoProbe Prodigy型核磁気共鳴装置
(測定条件)
測定核:13C(125MHz)、測定モード:シングルパルスプロトンブロードバンドデカップリング、パルス幅:45°(5.00μ秒)、ポイント数:64k、測定範囲:250ppm(−55〜195ppm)、繰り返し時間:5.5秒、積算回数:512回、測定溶媒:オルトジクロロベンゼン/ベンゼン−d6(4/1 v/v)、試料濃度:ca.60mg/0.6mL、測定温度:120℃、ウインドウ関数:exponential(BF:1.0Hz)、ケミカルシフト基準:ベンゼン−d6(128.0ppm)。
エチレン・α−オレフィン共重合体の融点は、インジウム標準にて較正したSII社製示差走査型熱量計(X−DSC7000)を用いて、以下のようにして測定した。
<High Temperature High Shear(HTHS)粘度>
潤滑油組成物のHTHS粘度(150℃)は、ASTM D4683に基づき、150℃、106s-1で測定した。なお、HTHS粘度は、SAE粘度分類によって、エンジン保護のための下限粘度が規定されている。したがって、潤滑油組成物の省燃費性の優劣を確認するため、HTHS粘度が同程度となるよう配合を行い、潤滑油組成物の各種粘度特性を比較した。
潤滑油組成物の100℃における動粘度(KV)を、ASTM D445に基づいて測定した。なお、HTHS粘度が同程度の潤滑油組成物を比較した場合、潤滑油組成物の前記動粘度が小さいほど、潤滑油組成物は、高温時の省燃費性に優れる。一方で、動粘度が低すぎると、潤滑性に劣ることがある。これらのバランスを満足させるためには動粘度が特定の範囲にあることが望ましい場合がある。
潤滑油組成物のCCS粘度(−35℃)を、ASTM D5393に基づいて測定した。CCS粘度は、クランク軸における低温での摺動性(始動性)の評価に用いられる。CCS粘度が小さいほど、潤滑油の低温粘度(低温特性)が優れることを示す。なお、HTTSが同程度の潤滑油組成物を比較した場合、潤滑油組成物のCCS粘度が小さいほど、潤滑油組成物は、低温時の省燃費性(低温始動性)に優れる。
潤滑油組成物のSSIを、JPI−5S−29−88規定を参考にした超音波法で測定した。潤滑油組成物に超音波を照射し、照射前後の動粘度低下率からSSIを測定した。SSIは潤滑油中の共重合体成分が摺動下で剪断力を受け分子鎖が切断することによる動粘度の低下の尺度である。SSIが大きい値であるほど、動粘度の低下が大きいことを示す。
US−300TCVP型超音波剪断安定度試験装置(プリムテック製)
(測定条件)
発振周波数:10KHz
試験温度:40℃
照射ホーン位置:液面下2mm
(測定方法)
試料容器に試料を30ml採取し、4.2Vの出力電圧により超音波を30分間照射する。超音波照射前後の試料油の100℃における動粘度を測定し、以下に示す式により、SSIを求める。
Vo:超音波照射前の100℃動粘度(mm2/s)
Vs:超音波照射後の100℃動粘度(mm2/s)
Vb:潤滑油用粘度調整剤の成分量(下記重合例で得たエチレン・α−オレフィン共重合体)を0質量%として調整した潤滑油組成物またはエンジン油(潤滑油組成物)の100℃動粘度(mm2/s)
[重合例1A、1B]
以下、エチレン・α−オレフィン共重合体の重合例について記載する。なお、分析および潤滑油調整剤評価に必要な量を確保するため、複数回の重合を実施していることがある。
表2Aに記載したとおりに重合条件を変更したこと以外は重合例1Aと同様に行った。ただし、重合例7Aおよび8Aでは、上記化合物(1)のヘキサン溶液(0.038mmol/L)、Ph3CB(C6F5)4のヘキサン溶液(0.30mmol/L)、iBu3Alのヘキサン溶液(5.0mmol/L)を用いた。
表2−1Bおよび2−2Bに記載したとおりに重合条件を変更したこと以外は重合例1Bと同様に行った。ただし、重合例6Bでは、上記化合物(1)のヘキサン溶液(0.038mmol/L)、Ph3CB(C6F5)4のヘキサン溶液(0.30mmol/L)、iBu3Alのヘキサン溶液(5.0mmol/L)を用いた。また、重合例21Bおよび22Bでは、上記化合物(1)のヘキサン溶液(0.015mmol/L)、Ph3CB(C6F5)4のヘキサン溶液(1.2mmol/L)、iBu3Alのヘキサン溶液(5.0mmol/L)を用いた。また、プロピレンの代わりに、重合例7B〜13Bではブテン-1を、重合例14B〜20Bではオクテン-1を、重合例21Bおよび22Bでは4-メチル-ペンテン-1をコモノマーとして使用した。
上記の重合例で得られたエチレン・プロピレン共重合体を潤滑油用粘度調整剤として用いて、潤滑油組成物を調製した。潤滑油組成物の150℃におけるHTHSが2.6mPa・s程度になるように、エチレン・プロピレン共重合体の添加量を調整した。
添加剤*:8.64質量%
流動点降下剤:0.3質量%
(ポリメタクリレート「ルブラン165」、東邦化学工業社製)
エチレン・プロピレン共重合体:0.53〜2.92質量%(表3Aに示すとおり)
合計 100.0(質量%)
注(*) 添加剤=CaおよびNaの過塩基性清浄剤、N含有分散剤、アミン性[aminic]およびフェノール性の酸化防止剤、ジアルキルジチオリン酸亜鉛類、摩擦調整剤、および消泡剤を含む従来のGF−5用エンジン油用添加剤パッケージ。
上記の重合例で得られたエチレン・α−オレフィン共重合体を潤滑油用粘度調整剤として用いて、潤滑油組成物を調製した。潤滑油組成物の150℃におけるHTHSが2.6mPa・s程度になるように、エチレン・α−オレフィン共重合体の添加量を調整した。
添加剤*:8.64質量%
流動点降下剤:0.3質量%
(ポリメタクリレート「ルブラン165」、東邦化学工業社製)
エチレン・α−オレフィン共重合体:0.63〜1.44質量%(表3Bに示すとおり)
合計 100.0(質量%)
注(*) 添加剤=CaおよびNaの過塩基性清浄剤、N含有分散剤、アミン性[aminic]およびフェノール性の酸化防止剤、ジアルキルジチオリン酸亜鉛類、摩擦調整剤、および消泡剤を含む従来のGF−5用エンジン油用添加剤パッケージ。
Claims (11)
- エチレン由来の構成単位の含有割合が70〜90モル%であり、極限粘度[η]が0.3〜1.0dl/gであるエチレン・α−オレフィン共重合体(A)を含有する潤滑油組成物。
- 前記共重合体(A)が、エチレン由来の構成単位の含有割合が70モル%を超えて90モル%以下であり、極限粘度[η]が0.3〜1.0dl/gである、エチレンと炭素数4以上のα−オレフィンとの共重合体である請求項1に記載の潤滑油組成物。
- 前記共重合体(A)が、示差走査型熱量計(DSC)で測定した融点が100℃以下であるかまたは融点が観測されない共重合体である請求項1または2に記載の潤滑油組成物。
- 潤滑油基油(B)をさらに含有する請求項1〜3のいずれか1項に記載の潤滑油組成物。
- エンジン油である請求項1〜4のいずれか1項に記載の潤滑油組成物。
- エチレン由来の構成単位の含有割合が70モル%を超えて90モル%以下であり、極限粘度[η]が0.3〜1.0dl/gである、エチレンと炭素数4以上のα−オレフィンとの共重合体を含有する潤滑油用粘度調整剤。
- 100℃における動粘度が7.4〜14.7mm2/sであり、エンジン用である請求項1に記載の潤滑油組成物。
- 前記共重合体(A)が、示差走査型熱量計(DSC)で測定した融点が100℃以下であるかまたは融点が観測されない共重合体であり、
エンジン用である
請求項1または7に記載の潤滑油組成物。 - 前記共重合体(A)において、エチレン由来の構成単位の含有割合が79〜90モル%であり、
エンジン用である
請求項1、7または8に記載の潤滑油組成物。 - 潤滑油基油(B)をさらに含有し、
エンジン用である
請求項1、7〜9のいずれか1項に記載の潤滑油組成物。 - エチレン由来の構成単位の含有割合が79〜90モル%であり、極限粘度[η]が0.3〜1.0dl/gであるエチレン・α−オレフィン共重合体を含有する、エンジン用潤滑油のための粘度調整剤。
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