JP7379343B2 - 高分子無機ナノ粒子組成物、それらの製造方法、及び潤滑剤としてのそれらの使用 - Google Patents
高分子無機ナノ粒子組成物、それらの製造方法、及び潤滑剤としてのそれらの使用 Download PDFInfo
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- JP7379343B2 JP7379343B2 JP2020540593A JP2020540593A JP7379343B2 JP 7379343 B2 JP7379343 B2 JP 7379343B2 JP 2020540593 A JP2020540593 A JP 2020540593A JP 2020540593 A JP2020540593 A JP 2020540593A JP 7379343 B2 JP7379343 B2 JP 7379343B2
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Description
本発明は潤滑の分野に関する。潤滑剤は、表面間の摩擦を低減する組成物である。潤滑剤は、2つの表面間の運動の自由を可能にし、かつ表面の機械的摩耗を低減することに加えて、表面の腐食を抑制し、及び/又は熱もしくは酸化による表面への損傷を抑制しうる。潤滑剤組成物の例は、エンジンオイル、トランスミッション液、ギアオイル、工業用潤滑油、グリース及び金属加工油を含むが、これらに制限されない。
徹底的な調査の結果、本発明の発明者らは、驚くべきことに、請求項1において本発明の第一の態様として定義した高分子無機ナノ粒子組成物が、潤滑油中で非常に良好に分散しながら潤滑剤組成物に添加される場合に改善された極圧性能及び減摩性能を提供することを見出している。
本発明による高分子無機ナノ粒子組成物
本発明による高分子無機ナノ粒子組成物は、1つ以上の層間化合物(A)と1つ以上のポリマー化合物(B)とを含む混合物を粉砕することによって得られることを特徴とし、ここで
(A) 1つ以上の層間化合物は、分子式MX2を有する金属カルコゲニドを含み、式中、Mは、チタン(Ti)、バナジウム(V)、クロム(Cr)、マンガン(Mn)、鉄(Fe)、コバルト(Co)、ニッケル(Ni)、銅(Cu)、亜鉛(Zn)、ジルコニウム(Zr)、ニオブ(Nb)、モリブデン(Mo)、テクネチウム(Tc)、ルテニウム(Ru)、ロジウム(Rh)、パラジウム(Pd)、銀(Ag)、カドミウム(Cd)、ハフニウム(Hf)、タンタル(Ta)、タングステン(W)、レニウム(Re)、オスミウム(Os)、イリジウム(Ir)、白金(Pt)、金(Au)、水銀(Hg)及びそれらの組合せからなる群から選択される金属元素であり、Xは、硫黄(S)、セレン(Se)、テルル(Te)、酸素(O)及びそれらの組合せからなる群から選択されるカルコゲン元素であり、
かつ
(B) 1つ以上のポリマー化合物は、以下、
a) 以下、
a1) ヒドロキシアルキル(メタ)アクリレート、例えば3-ヒドロキシプロピル(メタ)アクリレート、3,4-ジヒドロキシブチル(メタ)アクリレート、2-ヒドロキシエチル(メタ)アクリレート、2-ヒドロキシプロピル(メタ)アクリレート、2,5-ジメチル-1,6-ヘキサンジオール(メタ)アクリレート、1,10-デカンジオール(メタ)アクリレート、
a2) アミノアルキル(メタ)アクリレート及びアミノアルキル(メタ)アクリルアミド、例えばN-(3-ジメチル-アミノプロピル)メタクリルアミド、3-ジエチルアミノペンチル(メタ)アクリレート、3-ジブチル-アミノヘキサデシル(メタ)アクリレート、
a3) メタ)アクリル酸のニトリル及び他の窒素含有(メタ)アクリレート、例えばN-(メタクリロイルオキシエチル)ジイソブチルケチミン、N-(メタクリロイルオキシエチル)ジヘキサデシル-ケチミン、(メタ)アクリロイルアミドアセトニトリル、2-メタクリロイルオキシエチルメチルシアナミド、シアノメチル(メタ)アクリレート、
a4) アリール(メタ)アクリレート、例えばベンジル(メタ)アクリレート又はフェニル(メタ)アクリレート、ここでそれぞれの場合のアクリル残基は、非置換であるか又は4回まで置換されていてよい、
a5) カルボニル含有(メタ)アクリレート、例えば2-カルボキシエチル(メタ)アクリレート、カルボキシメチル(メタ)アクリレート、N-メチルアクリロイルオキシ)-ホルムアミド、アセトニル(メタ)アクリレート、N-メタクリロイル-2-ピロリジノン、N-(2-メチルアクリロキシオキシエチル)-2-ピロリジノン、N-(3-メタクリロイルオキシ-プロピル)-2-ピロリジノン、N-(2-メタクリロイルオキシペンタデシル)-2-ピロリジノン、N-(3-メタクリロイルオキシヘプタデシル)-2-ピロリジノン、
a6) エーテルアルコールの(メタ)アクリレート、例えばテトラヒドロフルフリル(メタ)アクリレート、メトキシエトキシエチル(メタ)アクリレート、1-ブトキシプロピル(メタ)アクリレート、シクロヘキシルオキシエチル(メタ)アクリレート、プロポキシエトキシエチル(メタ)アクリレート、ベンジルオキシエチル(メタ)アクリレート、フルフリル(メタ)アクリレート、2-ブトキシエチル(メタ)アクリレート、2-エトキシ-2-エトキシエチル(メタ)アクリレート、2-メトキシ-2-エトキシプロピル(メタ)アクリレート、エトキシル化(メタ)アクリレート、1-エトキシブチル(メタ)アクリレート、メトキシエチル(メタ)アクリレート、2-エトキシ-2-エトキシ-2-エトキシエチル(メタ)アクリレート、(メタ)アクリル酸及びメトキシポリエチレングリコールのエステル、
a7) ハロゲン化アルコールの(メタ)アクリレート、例えば2,3-ジブロモプロピル(メタ)アクリレート、4-ブロモフェニル(メタ)アクリレート、1,3-ジクロロ-2-プロピル(メタ)アクリレート、2-ブロモエチル(メタ)アクリレート、2-ヨードエチル(メタ)アクリレート、クロロメチル(メタ)アクリレート、
a8) オキシラニル(メタ)アクリレート、例えば2,3-エポキシブチル(メタ)アクリレート、3,4-エポキシブチル(メタ)アクリレート、10,11-エポキシウンデシル(メタ)アクリレート、2,3-エポキシシクロヘキシル(メタ)アクリレート、オキシラニル(メタ)アクリレート、例えば10,11-エポキシヘキサデシル(メタ)アクリレート、グリシジル(メタ)アクリレート、
a9) リン含有、ホウ素含有、及び/又はケイ素含有(メタ)アクリレート、例えば2-(ジメチル-ホスファト)プロピル(メタ)アクリレート、2-(エチルホスフィト)プロピル(メタ)アクリレート、2-ジメチルホスフィノメチル(メタ)アクリレート、ジメチルホスホノエチル(メタ)アクリレート、ジエチルメタクリロイルホスホネート、ジプロピルメタクリロイルホスフェート、2-(ジブチルホスホノ)エチル(メタ)アクリレート、2,3-ブチレンメタクリロイルエチルボレート、メチルジエトキシメタクリロイルエトキシシラン、ジエチルホスファトエチル(メタ)アクリレート;
a10) 硫黄含有(メタ)アクリレート、例えばエチルスルフィニルエチル(メタ)アクリレート、4-チオ-シアネートブチル(メタ)アクリレート、エチルスルホニルエチル(メタ)アクリレート、チオシアネートメチル(メタ)アクリレート、メチルスルフィニルメチル(メタ)アクリレート、ビス(メタクリロイルオキシエチル)スルフィド、
a11) 複素環式(メタ)アクリレート、例えば2-(1-イミダゾリル)エチル(メタ)アクリレート、オキサゾリジニルエチル(メタ)アクリレート、N-メタクリロイルモルホリン及び2-(4-モルホリニル)エチル(メタ)アクリレート、
a12) マレイン酸及びマレイン酸誘導体、例えばマレイン酸のモノエステル及びジエステル、マレイン酸無水物、メチルマレイン酸無水物、マレインイミド、メチルマレインイミド、
a13) フマル酸及びフマル酸誘導体、例えばフマル酸のモノエステル及びジエステル、
a14) ハロゲン化ビニル、例えば塩化ビニル、フッ化ビニル、塩化ビニリデン及びフッ化ビニリデン、
a15) ビニルエステル、例えば酢酸ビニル、
a16) 芳香族基を含有するビニルモノマー、例えばスチレン、側鎖にアルキル置換基を有する置換スチレン、例えばアルファ-メチルスチレン及びアルファ-エチルスチレン、環上でアルキル置換基を有する置換スチレン、例えばビニルトルエン及びp-メチルスチレン、ハロゲン化スチレン、例えばモノクロロスチレン、ジクロロスチレン、トリブロモスチレン及びテトラブロモスチレン、
a17) 複素環式ビニル化合物、例えば2-ビニルピリジン、3-ビニルピリジン、2-メチル-5-ビニルピリジン、3-エチル-4-ビニルピリジン、2,3-ジメチル-5-ビニルピリジン、ビニルピリミジン、ビニルピペリジン、9-ビニルカルバゾール、3-ビニルカルバゾール、4-ビニルカルバゾール、1-ビニルイミダゾール、2-メチル-1-ビニルイミダゾール、N-ビニルピロリドン、2-ビニルピロリドン、N-ビニルピロリジン、3-ビニルピロリジン、N-ビニルカプロラクタム、N-ビニルブチロラクタム、ビニルオキソラン、ビニルフラン、ビニルチオフェン、ビニルチオラン、ビニルチアゾール及び水素化ビニルチアゾール、ビニルオキサゾール及び水素化ビニルオキサゾール、
a18) ビニル及びイソプレニルエーテル、
a19) メタクリル酸及びアクリル酸、
を含むリストから選択される、成分a)として1つ以上の官能性モノマー、
並びに
b) 1つ以上のアルキル(メタ)アクリレートモノマー、及び
c) (メタ)アクリル酸の1つ以上のエステルと、数平均分子量(Mn)500~10000g/molを有する1つ以上のヒドロキシル化水素化ポリブタジエンとの反応生成物
からなるリストから選択される1つ又は双方の成分
を含むモノマー組成物を重合することによって得られ、かつ
1つ以上の層間化合物(A)と1つ以上のポリマー化合物(B)との質量比は、20:1~1:5である。
本発明による層間化合物という用語は、要素又は層の間に挿入することができる化合物を表す。層間化合物は、典型的にフラーレン状の形態を有する。フラーレン状の形態のコアは、中空、中実、非晶質、又はそれらの組合せであってよい。フラーレン状の形態は、カゴの形態を有することにもあてはまる。より詳述すれば、いくつかの実施形態において、無機フラーレン状の形態を有する層間化合物は、そのコアで中空又は中実であり、かつその周囲で層状であるカゴの形態であってよい。例えば、無機フラーレン状の形態を有する層間化合物は、単層又は二重層構造であってよい。層間化合物は、任意の数の層を有してよいため、単層又は二重層構造のみに制限されない。これらの構造は、当該技術分野においてネスト化層構造ともいわれる。
本発明の好ましい実施形態において、1つ以上のポリマー化合物(B)は、成分a)及びb)を含むが、成分c)を含んでいないモノマー組成物を重合することによって得られ、その際、1つ以上のポリマー化合物(B)は、5000~300000g/mol、より好ましくは10000~200000g/molの質量平均分子量(Mw)を有する。
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは2~40質量%、最も好ましくは3~35質量%の成分a)として1つ以上の官能性モノマー、及び
b)1つ以上のポリマー化合物(B)に対して、10~99質量%、好ましくは20~98質量%、より好ましくは30~98質量%、最も好ましくは35~97質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、及び
c)1つ以上のポリマー化合物(B)に対して、0~89質量%、好ましくは10~80質量%、より好ましくは20~70質量%、最も好ましくは25~60質量%の、成分c)として1つ以上の(メタ)アクリル酸のエステルと500~10000g/molの数平均分子量(Mn)を有する1つ以上のヒドロキシル化水素化ポリブタジエンとの反応生成物。
「C1-40アルキル(メタ)アクリレート」という用語は、(メタ)アクリル酸と、炭素原子1~40個を有する直鎖、環状又は分枝鎖のアルコールとのエステルをいう。この用語は、特定の長さのアルコールを有する個々の(メタ)アクリル酸エステル、及び同様に(メタ)アクリル酸エステルと異なる長さのアルコールとの混合物を包含する。
b1)式(I)
b2)式(II)
b3)式(III)
本発明に従って成分c)として使用するための1つ以上のヒドロキシル化水素化ポリブタジエンは、500g/mol~10000g/molの数平均分子量Mnを有する。それらの高分子量の理由から、ヒドロキシル化水素化ポリブタジエンは、本発明の記載内容においてマクロアルコールともいうことができる。(メタ)アクリル酸の対応するエステルは、本発明の記載内容においてマクロモノマーともいうことができる。
本発明に従って、請求項1で定義した1つ以上のポリマー化合物(B)は、以下を含むモノマー組成物を重合することによって得られることが好ましい:
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは2~40質量%、最も好ましくは3~35質量%の成分a)として1つ以上の官能性モノマー、及び
b)1つ以上のポリマー化合物(B)に対して、10~99質量%、好ましくは20~98質量%、より好ましくは30~98質量%、最も好ましくは35~97質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、及び
c)1つ以上のポリマー化合物(B)に対して、0~89質量%、好ましくは10~80質量%、より好ましくは20~70質量%、最も好ましくは25~60質量%の、成分c)として1つ以上の(メタ)アクリル酸のエステルと500~10000g/molの数平均分子量(Mn)を有する1つ以上のヒドロキシル化水素化ポリブタジエンとの反応生成物。
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは2~40質量%、最も好ましくは3~35質量%の成分a)として1つ以上の官能性モノマー、及び
b)1つ以上のポリマー化合物(B)に対して、40~99質量%、好ましくは50~98質量%、より好ましくは60~98質量%、最も好ましくは65~97質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは2~40質量%、最も好ましくは3~35質量%の成分a)として1つ以上の官能性モノマー、及び
b1)1つ以上のポリマー化合物(B)に対して、0~50質量%、好ましくは0~40質量%、より好ましくは0~20質量%、最も好ましくは0~10質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、及び
b2)1つ以上のポリマー化合物(B)に対して、40~99質量%、好ましくは50~98質量%、より好ましくは60~98質量%、最も好ましくは65~97質量%の、成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは5~40質量%、最も好ましくは5~25質量%の成分a)として1つ以上の官能性モノマー、及び
b)1つ以上のポリマー化合物(B)に対して、10~95質量%、好ましくは20~80質量%、より好ましくは30~70質量%、最も好ましくは35~60質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、及び
c)1つ以上のポリマー化合物(B)に対して、1~89質量%、好ましくは10~80質量%、より好ましくは20~70質量%、最も好ましくは25~60質量%の、成分c)として1つ以上の(メタ)アクリル酸のエステルと500~10000g/molの数平均分子量(Mn)を有する1つ以上のヒドロキシル化水素化ポリブタジエンとの反応生成物、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは2~40質量%、最も好ましくは3~35質量%の、モノマーa2)、a3)、a5)、a11)、a17)又はそれらの混合物からなる群から選択される成分a)として1つ以上の官能性モノマー、及び
b)1つ以上のポリマー化合物(B)に対して、40~99質量%、好ましくは50~98質量%、より好ましくは60~98質量%、最も好ましくは65~97質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a2)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは2~40質量%、最も好ましくは3~35質量%の成分a)として1つ以上の官能性モノマーa2)、及び
b)1つ以上のポリマー化合物(B)に対して、40~99質量%、好ましくは50~98質量%、より好ましくは60~98質量%、最も好ましくは65~97質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a2)1つ以上のポリマー化合物(B)に対して、1~10質量%の成分a)としてアミノアルキル(メタ)アクリルアミド、最も好ましくはN-(3-ジメチル-アミノプロピル)メタクリルアミド、
b1)1つ以上のポリマー化合物(B)に対して、0~10質量%の第一の成分b)として式(I)のアルキル(メタ)アクリレートモノマー、最も好ましくはメチルメタクリレート、
b2)1つ以上のポリマー化合物(B)に対して、80~99質量%の成分b)として式(II)のアルキル(メタ)アクリレートモノマー、最も好ましくはラウリルメタクリレート、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a2)1つ以上のポリマー化合物(B)に対して、1~10質量%の成分a)としてアミノアルキル(メタ)アクリルアミド、最も好ましくはN-(3-ジメチル-アミノプロピル)メタクリルアミド、及び
b2)1つ以上のポリマー化合物(B)に対して、90~99質量%の成分b)として式(II)のアルキル(メタ)アクリレートモノマー、最も好ましくはラウリルメタクリレート、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a2)1つ以上のポリマー化合物(B)に対して、1~10質量%の成分a)としてアミノアルキル(メタ)アクリルアミド、最も好ましくはN-(3-ジメチル-アミノプロピル)メタクリルアミド、
b1)1つ以上のポリマー化合物(B)に対して、1~10質量%の第一の成分b)として式(I)のアルキル(メタ)アクリレートモノマー、最も好ましくはメチルメタクリレート、及び
b2)1つ以上のポリマー化合物(B)に対して、80~98質量%の第二の成分b)として式(II)のアルキル(メタ)アクリレートモノマー、最も好ましくはC12~C15メタクリレート、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは5~40質量%、最も好ましくは5~25質量%のモノマーa2)、a3)、a5)、a11)、a16)、a17)又はそれらの混合物からなる群から選択される成分a)として1つ以上の官能性モノマー、及び
b)1つ以上のポリマー化合物(B)に対して、10~95質量%、好ましくは20~80質量%、より好ましくは30~70質量%、最も好ましくは35~60質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、及び
c)1つ以上のポリマー化合物(B)に対して、1~89質量%、好ましくは10~80質量%、より好ましくは20~70質量%、最も好ましくは25~60質量%の、成分c)として1つ以上の(メタ)アクリル酸のエステルと500~10000g/molの数平均分子量(Mn)を有する1つ以上のヒドロキシル化水素化ポリブタジエンとの反応混生成物、
ここで、モノマー組成物のモノマーの量は、合計で100質量%になる。
a2)1つ以上のポリマー化合物(B)に対して、0.5~5質量%の第一の成分a)としてアミノアルキル(メタ)アクリルアミド、最も好ましくはN-(3-ジメチル-アミノプロピル)メタクリルアミド、
a16)1つ以上のポリマー化合物(B)に対して、5~20質量%の第二の成分a)として芳香族基を含むビニルモノマー、最も好ましくはスチレン、
b1)1つ以上のポリマー化合物(B)に対して、25~60質量%の第一の成分b)として式(I)のアルキル(メタ)アクリレートモノマー、最も好ましくはメチルメタクリレート及び/又はブチルメタクリレート、
b2)1つ以上のポリマー化合物(B)に対して、1~10質量%の第二の成分b)として式(II)のアルキル(メタ)アクリレートモノマー、最も好ましくはラウリルメタクリレート、及び
c)1つ以上のポリマー化合物(B)に対して、25~60質量%の成分c)として(メタ)アクリル酸と500~10000g/molの数平均分子量(Mn)を有するヒドロキシル化水素化ポリブタジエンとのエステル、最も好ましくは(メタ)アクリル酸と1500~5000g/molの数平均分子量(Mn)を有するヒドロキシル化水素化ポリブタジエンとのエステルの反応に由来するマクロモノマー、
ここで、モノマー組成物の全てのモノマーの量は、合計で100質量%になる。
化合物(B)は、前記の好ましいモノマー組成物の1つで調製される。
本発明に従って、前記ポリマーは、以下
(a)前記モノマー組成物を準備するステップ、及び
(b)モノマー組成物中でラジカル重合を開始するステップ
を含む方法によって調製されうる。
高分子無機ナノ粒子組成物における本発明に従って、1つ以上の層間化合物(A)と1つ以上のポリマー化合物(B)との質量比は、20:1~1:5、好ましくは10:1~1:2、より好ましくは5:1~1:1、最も好ましくは4:1~2:1である。
a)1つ以上のポリマー化合物(B)に対して、1~60質量%、好ましくは2~50質量%、より好ましくは2~40質量%、最も好ましくは3~35質量%の成分a)として1つ以上の官能性モノマー、及び
b)1つ以上のポリマー化合物(B)に対して、10~99質量%、好ましくは20~98質量%、より好ましくは30~98質量%、最も好ましくは35~97質量%の成分b)として1つ以上のアルキル(メタ)アクリレートモノマー、及び
c)1つ以上のポリマー化合物(B)に対して、0~89質量%、好ましくは10~80質量%、より好ましくは20~70質量%、最も好ましくは25~60質量%の、成分c)として1つ以上の(メタ)アクリル酸のエステルと500~10000g/molの数平均分子量(Mn)を有する1つ以上のヒドロキシル化水素化ポリブタジエンとの反応生成物、
を含むモノマー組成物を重合することによって得られ、
ここで、1つ以上の層間化合物(A)と1つ以上のポリマー化合物(B)との質量比は、20:1~1:5、好ましくは10:1~1:2、より好ましくは5:1~1:1、最も好ましくは4:1~2:1である。
(a)本明細書において定義される1つ以上の層間化合物(A)を準備するステップ、
(b)本明細書において定義される1つ以上のポリマー化合物(B)を準備するステップ、
(c)好ましくは、本明細書において定義される溶媒(C)を準備するステップ、
(d)少なくとも1つ以上の層間化合物(A)と1つ以上のポリマー化合物(B)とを合して混合物を得るステップ、好ましくは少なくとも1つ以上の層間化合物(A)と1つ以上のポリマー化合物(B)と溶媒(C)とを合して混合物を得るステップ、及び
(e)混合物を粉砕するステップ
を含む。
本発明のさらなる態様は、潤滑剤組成物のための添加剤としての本明細書において定義した高分子無機ナノ粒子組成物の使用である。
本発明のさらに他の態様は、以下を含む組成物である:
(i)基油、及び
(ii)本明細書において定義される高分子無機ナノ粒子組成物。
本発明は、本発明の範囲を制限することを意図することなく、実施例及び比較例に関して以下にさらに詳細に説明される。
C1AMA C1-アルキルメタクリレート(メチルメタクリレート;MMA)
C4AMA C4-アルキルメタクリレート(n-ブチルメタクリレート)
C12-14AMA C12-14-アルキルメタクリレート
C12-15AMA C12-15-アルキルメタクリレート
OCTMO オクチルトリメトキシシラン
DMAPMAA N-3-ジメチルアミノプロピルメタクリルアミド
fbranch mol%での分枝度
MA-1 マクロアルコール(ヒドロキシル化水素化ポリブタジエンMn=2000g/mol)
MM-1 メタクリレート官能基を有するMA-1のマクロモノマー
Mn 数平均分子量
Mw 質量平均分子量
NB3020 Nexbase(登録商標)3020、2.2cStのKV100を有するNeste社製の群IIIの基油
NB3043 Nexbase(登録商標)3043、4.3cStのKV100を有するNeste社製の群IIIの基油
NB3060 Nexbase(登録商標)3060、6.0cStのKV100を有するNeste社製の群IIIの基油
VISCOBASE 5-220 480cStのKV100を有するEvonik社製の群Vの合成基流体
VISCOPLEX 14-520 消泡剤
DIパッケージ Afton HiTec(登録商標)307(洗浄剤抑制剤)
PPD 流動点降下剤
PDI 多分散指数、Mw/Mnにより算出した分子量分布
MTM ミニトラクション機械装置。
マクロアルコールを、20~45℃で1,3-ブタジエンとブチルリチウムとをアニオン重合することによって合成した。所望の重合度に達したら、プロピレンオキシドを添加することにより反応を停止し、そしてメタノールを用いた沈殿によりリチウムを除去した。続いて、水素雰囲気下で、貴金属触媒の存在下に、最高140℃及び圧力200barでポリマーを水素化した。水素化が終了した後に、貴金属触媒を除去し、そして有機溶媒を減圧下で除去して、100%マクロアルコールMA-1を得た。
サーベル型攪拌機(saber stirrer)、空気入口管、コントローラー付き熱電対、加熱マントル、3mmワイヤースパイラルのランダムパッキングを有するカラム、蒸気分割機、上部温度計、還流冷却器、及び基体冷却器を備えた2Lの攪拌装置中で、前記マクロモノマー1000gを、60℃で攪拌することにより、メタクリル酸メチル(MMA)中で溶解した。その溶液に、2,2,6,6-テトラメチルピペリジン-1-オキシルラジカル20ppm及びヒドロキノンモノメチルエーテル200ppmを添加する。安定化のために空気を通過させながらMMAの還流(最低温度約110℃)まで加熱した後に、共沸乾燥のためにMMA約20mLを蒸留する。95℃に冷却した後に、LiOCH3を添加し、そしてその混合物を加熱して還流する。約1時間の反応時間の後に、メタノールの形成により、頂部温度は~64℃まで下がる。約100℃の一定の最高温度を再び確立するまで、形成したメタノール/MMA共沸混合物を常に蒸留する。この温度で、混合物をさらに1時間反応させる。さらに後処理するために、大部分のMMAを減圧下で抜き取る。不溶性の触媒残留物を、圧力濾過(Seitz T1000 depth filter)により除去する。
前述したように、ポリメチルメタクリレート(PMMA)標準を使用して較正したゲル浸透クロマトグラフィー(GPC)によってポリマーの質量平均分子量を測定した。溶出液としてテトラヒドロフラン(THF)を使用する。
Nexbase 3043 200グラム、n-3-ジメチルアミノプロピルメタクリルアミド(DMAPMAA)11.34グラム、ラウリルメタクリレート(C12-14AMA)272.21グラム、n-ドデシルメルカプタン(n-DDM)5.53グラム、2-エチルヘキシルチオグリコレート(TGEH)5.53グラムを、2リットルの四ツ口丸底フラスコに装入した。その反応混合物を、C攪拌棒を使用して攪拌し、窒素で不活性化し、そして90℃に加熱した。反応混合物が設定温度に達したら、t-ブチルペルオクトエート2.83グラムを、2時間にわたって反応器に供給した。2時間後に、その混合物を100℃まで加熱し、そして設定値に達した後に、t-ブチルペル-2-エチルヘキサノエート1.42グラム及びtert-ブチルペルピバレート1.13グラムを1時間で供給した。残留モノマーを、良好なモノマー変換を確実にするためにガスクロマトグラフィーによって測定した。得られたポリマーは、質量平均分子量Mw10500g/mol(PMMA標準)を有する。
100Nオイル(群IIオイル)276グラム、メチルメタクリレート16グラム、ジメチルアミノプロピルメタクリルアミド13グラム、C12-15AMA290グラム、及びn-ドデシルメルカプタン0.5グラムを、2リットルの四ツ口丸底フラスコに装入した。その反応混合物を、C攪拌棒を使用して攪拌し、窒素で不活性化し、そして110℃に加熱した。反応混合物が設定温度に達したら、tert-ブチル-2-エチルペルオキシヘキサノエート0.6グラムを3時間にわたって反応器に供給した。供給が完了した後に、1時間攪拌して反応させた。残留モノマーを、良好なモノマー変換を確実にするためにガスクロマトグラフィーによって測定した。得られたポリマーは、質量平均分子量Mw157000g/mol(PMMA標準)を有する。
NB3020 85グラム、ベリラン230SPP 85グラム、マクロモノマー140グラム、ブチルメタクリレート107グラム、スチレン28グラム、ラウリルメタクリレート13グラム、ジメチルアミノプロピルメタクリルアミド8グラム、及びn-ドデシルメルカプタン1グラムを、2リットルの四ツ口丸底フラスコに装入した。その反応混合物を、C攪拌棒を使用して攪拌し、窒素で不活性化し、そして115℃に加熱した。反応混合物が設定温度に達したら、tert-ブチル-2-エチルペルオキシヘキサノエート0.9グラムを、3時間にわたって反応器に供給した。2,2-ジ-(tert-ブチルペルオキシ)-ブタン0.5グラムを、前の供給後30分及び3時間で添加した。1時間攪拌して反応させ、そして追加のNB3020 132グラムを反応器に添加して1時間混合させた。得られたポリマーは、質量平均分子量Mw260000g/mol(PMMA標準)を有する。
分散液IE1:
IF-WS2粒子4gを、P1 2gを含むNB3043オイル14gの溶液に加え、この混合物を超音波(400ワットを有する超音波プロセッサUP400S、Ti-sonotrodeで24kHz)で処理する。添加が完了した後に、分散液を120分間処理する。粒径分布(動的光散乱装置、LA-950、日本国在、Horiba Ltd.社製を使用してTegosoft DECオイルで測定)は、54nmのd50値を示す。
IF-WS2粒子4gを、P2 2.2gを含むNB3043オイル13.6gの溶液に添加し、この混合物を超音波(400ワットを有する超音波プロセッサUP400S、Ti-sonotrodeで24kHz)で処理する。添加が完了した後に、分散液を120分間処理する。粒径分布(動的光散乱装置、LA-950、日本国在、Horiba Ltd.社製を使用してTegosoft DECオイルで測定)は、71nmのd50値を示す。
ボールミル装置(Netzsch Laboratory Mill Micro Series、粉砕チャンバーの85%を0.4mmのY安定化ZrO2ボールで満たした)には、蠕動ポンプを80rpm及びボールミルを1000rpmに設定しながら、NB3043オイル245g及びP1 35gを予め装入する。その後、IF-WS2粒子70gをこの溶液に加える。ボールミルを回転速度3500rpmに設定し、そしてエネルギー1.0kWhを導入するまで分散液を処理する。粒径分布(動的光散乱装置、LA-950、日本国在、Horiba Ltd.社製を使用してTegosoft DECオイルで測定)は、47nmのd50値を示す。
ボールミル装置(Bachofen DynoMill、粉砕チャンバーの70%を0.3~0.6mmのCe安定化ZrO2ボールで満たした)に、ボールミルを1000rpmに設定しながら、NB3043オイル143.9g及びP2 24.1gを予め装入する。その後、IF-WS2粒子42gをこの溶液に加える。分散液を、エネルギー2.8kWhを導入するまで処理する。粒径分布(動的光散乱装置、LA-950、日本国在、Horiba Ltd.社製を使用してTegosoft DECオイルで測定)は、48nmのd50値を示す。
IF-WS2粒子4gを、P3 2.4gを含むNB3043オイル13.6gの溶液に加え、この混合物を超音波(400ワットを有する超音波プロセッサUP400S、Ti-sonotrodeで24kHz)で処理する。添加が完了した後に、分散液を120分間処理する。粒径分布(動的光散乱装置、LA-950、日本国在、Horiba Ltd.社製を使用してTegosoft DECオイルで測定)は、63nmのd50値を示す。
分散液CE1:
IF-WS2粒子4gを、ε-カプロラクタム1.2gを含むNB3043オイル14.8gの溶液に加え、この混合物を、それぞれ超音波(400ワットを有する超音波プロセッサUP400S、Ti-sonotrodeで24kHz)で120分間処理する。粒径分布(動的光散乱装置、LA-950、日本国在、Horiba Ltd.社製を使用してTegosoft DECオイルで測定)は、1427nmのd50値を示す。
IF-WS2粒子4gを、OCTMO1.2gを含むNB3043オイル14.8gの溶液に加え、この混合物を、それぞれ超音波(400ワットを有する超音波プロセッサUP400S、Ti-sonotrodeで24kHz)で120分間処理する。粒径分布(動的光散乱装置、LA-950、日本国在、Horiba Ltd.社製を使用してTegosoft DECオイルで測定)は、432nmのd50値を示す。
粒度分布を、Horiba Ltd.社製の動的光散乱装置LB-500を使用してTegosoft DECオイルで測定した。
潤滑配合物を、以下の表6に示される質量比に従って調製し、そしてそれらの摩擦及び融着の性能を、以下に記載した2つの方法を使用して試験した。記載した質量パーセントは、異なる配合物の全質量に基づく。
79.25質量% Nexbase(登録商標)3060(基油)
17.4質量% VISCOBASE(登録商標)5-220(基油)
0.7質量% PPD
2.65質量% Afton HiTec(登録商標)307(DIパッケージ)
+0.2質量% VISCOPLEX(登録商標)14-520(消泡剤)
DIN 51350第二部に従って4球融着試験を実施した(結果は図2を参照されたい)。
剪断安定性試験を、DIN 51350第6部に従って実施した。
摩擦係数を、以下の表4において記載した試験方法に従ってPCS Instruments社製のMTM2と名付けられたミニトラクション機械を使用して測定した。SRRは、滑り率(Sliding Roll Ratio)を示す。このパラメーターを2時間の試験中一定に維持し、(UBall-UDisc)/Uとして定義した。ここで、(UBall-UDisc)は滑り速度を示し、Uはエントレインメント速度を示し、U=(UBall+UDisc)/2で提供する。それぞれの試料についてのストライベック曲線(Stribeck curve)を、表8におけるプロトコルに従って測定した。
Claims (8)
- 潤滑剤組成物のための添加剤としての、溶媒(C)中の無機ナノ粒子の分散液の形態の高分子無機ナノ粒子組成物であって、
層間化合物(A)及び溶媒(C)としての基油中に溶解させた1つ以上のポリマー化合物(B)を含む混合物を粉砕することによって得られ、
(A) 層間化合物が、二硫化タングステンであり、かつ無機フラーレン状の形態を有し、
かつ
(B) 1つ以上のポリマー化合物は、
a2)1つ以上のポリマー化合物(B)の全質量に対して、0.5~5質量%の第一の成分a)としてアミノアルキル(メタ)アクリルアミド、
a16)1つ以上のポリマー化合物(B)の全質量に対して、5~20質量%の第二の成分a)としてスチレン、
b1) 1つ以上のポリマー化合物(B)の全質量に対して、25~60質量%の、第一の成分b)として式(I)
b2) 1つ以上のポリマー化合物(B)の全質量に対して、1~10質量%の、第二の成分b)として式(II)
及び
c)1つ以上のポリマー化合物(B)の全質量に対して、25~60質量%の、1つ以上の(メタ)アクリル酸のエステルと数平均分子量(Mn)1500~5000g/molを有する1つ以上のヒドロキシル化水素化ポリブタジエンとの反応生成物
を含むモノマー組成物を重合することにより得られ、モノマー組成物の全てのモノマーの量は、合計で100質量%になる、かつ
層間化合物(A)と1つ以上のポリマー化合物(B)との質量比が、4:1~2:1であり、
ここで、1つ以上のポリマー化合物(B)は、200000~500000g/molの質量平均分子量(Mw)を有する、前記高分子無機ナノ粒子組成物。 - 請求項1に記載の高分子無機ナノ粒子組成物を製造するための方法であって、
(a)層間化合物(A)を準備するステップ、
(b)1つ以上のポリマー化合物(B)を準備するステップ、
(c)溶媒(C)を準備するステップ、
(d)少なくとも層間化合物(A)と1つ以上のポリマー化合物(B)と溶媒(C)とを合して混合物を得るステップ、及び
(e)混合物を粉砕するステップ
を含む、前記方法。 - 少なくとも、層間化合物(A)、1つ以上のポリマー化合物(B)及び溶媒(C)を合して混合物を得る請求項2に記載の方法であって、ステップ(e)は、0.1~10kWh/kgのエネルギーを混合物に導入するボールミルプロセスを介して混合物を粉砕することを含む方法。
- 潤滑剤組成物のための添加剤としての、請求項1に記載の高分子無機ナノ粒子組成物の使用。
- 以下、
(a)基油、及び
(b)請求項1に記載の高分子無機ナノ粒子組成物
を含む、配合物。 - 基油が、API群Iの基油、API群IIの基油、API群IIIの基油、API群IVの基油、及びAPI群Vの基油、又はそれら基油の2つ以上の混合物からなるリストから選択される、請求項5に記載の配合物。
- 配合物の全質量に対して、(i)基油40~95質量%、及び(ii)高分子無機ナノ粒子組成物5~60質量%を含む、請求項5又は6に記載の配合物。
- 配合物の全質量に対して、(i)基油50~99.99質量%、及び(ii)高分子無機ナノ粒子組成物0.01~50質量%を含む、請求項5又は6に記載の配合物。
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BR102021017032A2 (pt) | 2021-08-27 | 2023-03-07 | Instituto Hercílio Randon | Preparado de nanopartículas de tântalo, uso e processo para sua obtenção |
CN114231342B (zh) * | 2021-12-22 | 2022-08-05 | 金陵科技学院 | 一种含多元有机/无机杂化添加剂自修复润滑油 |
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US20200369977A1 (en) | 2020-11-26 |
KR20200110698A (ko) | 2020-09-24 |
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KR102587269B1 (ko) | 2023-10-11 |
US11198833B2 (en) | 2021-12-14 |
JP2021512188A (ja) | 2021-05-13 |
BR112020014972A2 (pt) | 2020-12-22 |
EP3743489B1 (en) | 2021-08-18 |
RU2020126869A (ru) | 2022-02-24 |
EP3743489A1 (en) | 2020-12-02 |
WO2019145298A1 (en) | 2019-08-01 |
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CA3089063A1 (en) | 2019-08-01 |
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