JPH03243696A - Low-noise urea grease composition - Google Patents
Low-noise urea grease compositionInfo
- Publication number
- JPH03243696A JPH03243696A JP3961290A JP3961290A JPH03243696A JP H03243696 A JPH03243696 A JP H03243696A JP 3961290 A JP3961290 A JP 3961290A JP 3961290 A JP3961290 A JP 3961290A JP H03243696 A JPH03243696 A JP H03243696A
- Authority
- JP
- Japan
- Prior art keywords
- grease
- noise
- low
- thickener
- greases
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000004519 grease Substances 0.000 title claims abstract description 65
- 239000000203 mixture Substances 0.000 title claims abstract description 23
- 239000004202 carbamide Substances 0.000 title claims abstract description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims description 18
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 17
- 239000002199 base oil Substances 0.000 claims abstract description 16
- 125000001117 oleyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])/C([H])=C([H])\C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 16
- -1 urea compound Chemical class 0.000 claims abstract description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 10
- 229910052744 lithium Inorganic materials 0.000 abstract description 10
- 239000000344 soap Substances 0.000 abstract description 10
- 239000002480 mineral oil Substances 0.000 abstract description 7
- 235000010446 mineral oil Nutrition 0.000 abstract description 7
- 239000004711 α-olefin Substances 0.000 abstract description 5
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 abstract description 3
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 abstract description 2
- 239000012188 paraffin wax Substances 0.000 abstract description 2
- 229920001296 polysiloxane Polymers 0.000 abstract description 2
- 125000002529 biphenylenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3C12)* 0.000 abstract 1
- 239000002562 thickening agent Substances 0.000 description 28
- 238000002156 mixing Methods 0.000 description 17
- 239000002245 particle Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 11
- XMKLTEGSALONPH-UHFFFAOYSA-N 1,2,4,5-tetrazinane-3,6-dione Chemical compound O=C1NNC(=O)NN1 XMKLTEGSALONPH-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 150000001412 amines Chemical class 0.000 description 7
- 125000005442 diisocyanate group Chemical group 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 5
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 4
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 4
- 238000009472 formulation Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 150000003973 alkyl amines Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000001050 lubricating effect Effects 0.000 description 3
- ICLCCFKUSALICQ-UHFFFAOYSA-N 1-isocyanato-4-(4-isocyanato-3-methylphenyl)-2-methylbenzene Chemical compound C1=C(N=C=O)C(C)=CC(C=2C=C(C)C(N=C=O)=CC=2)=C1 ICLCCFKUSALICQ-UHFFFAOYSA-N 0.000 description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 125000000753 cycloalkyl group Chemical group 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 description 2
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- BVVFUHROAFTSMG-UHFFFAOYSA-N 3-methylbutan-1-amine;pentan-1-amine Chemical compound CCCCCN.CC(C)CCN BVVFUHROAFTSMG-UHFFFAOYSA-N 0.000 description 1
- KLPPPIIIEMUEGP-UHFFFAOYSA-N 4-dodecylaniline Chemical compound CCCCCCCCCCCCC1=CC=C(N)C=C1 KLPPPIIIEMUEGP-UHFFFAOYSA-N 0.000 description 1
- PSVFJKXGYVCMGR-UHFFFAOYSA-N C(C)(C)N.C(C(C)C)N.C(CCC)N Chemical compound C(C)(C)N.C(C(C)C)N.C(CCC)N PSVFJKXGYVCMGR-UHFFFAOYSA-N 0.000 description 1
- QBVCURPNLGSYTD-UHFFFAOYSA-N C(C)C(CN)CCCC.C(CCCCCCCCCCC)N Chemical compound C(C)C(CN)CCCC.C(CCCCCCCCCCC)N QBVCURPNLGSYTD-UHFFFAOYSA-N 0.000 description 1
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000006059 cover glass Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- LQTKPYMTQDVLJC-UHFFFAOYSA-N cyclohexanamine;cyclopentanamine Chemical compound NC1CCCC1.NC1CCCCC1 LQTKPYMTQDVLJC-UHFFFAOYSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000010696 ester oil Substances 0.000 description 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- AOMBLMKCISVTDH-UHFFFAOYSA-N hexadecan-1-amine;tetradecan-1-amine Chemical compound CCCCCCCCCCCCCCN.CCCCCCCCCCCCCCCCN AOMBLMKCISVTDH-UHFFFAOYSA-N 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- BHRZNVHARXXAHW-UHFFFAOYSA-N sec-butylamine Chemical compound CCC(C)N BHRZNVHARXXAHW-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 230000000699 topical effect Effects 0.000 description 1
- 150000005691 triesters Chemical class 0.000 description 1
Landscapes
- Lubricants (AREA)
Abstract
Description
【発明の詳細な説明】
[産業上の利用分野]
本発明は、低騒音を要求される軸受に用いられるジウレ
アグリース組成物に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a diurea grease composition used in bearings that require low noise.
[従来の技術とその問題点]
近年の技術発展とユーザーの高級指向から家庭電気製品
、OA機器、さらには自動車部品などにおいては、その
本来的な機能向上とともに耳障りな騒音の低減が課題と
なっている。[Conventional technology and its problems] Due to recent technological developments and users' preference for luxury products, it has become a challenge to improve the inherent functionality of home appliances, OA equipment, and even automobile parts, as well as reduce harsh noise. ing.
この様な機器類の騒音の発生源の1つとして、モーター
など回転装置の回転軸を支えている軸受が挙げられる。One of the sources of noise in such equipment is bearings that support the rotating shafts of rotating devices such as motors.
この軸受から発生する音は、他の部分から発生する音と
一緒になって機器全体の騒音レベルを押し上げる事にな
る。この軸受騒音の原因としては、軸受の加工組立精度
、取り付は精度の問題、潤滑剤として使用するグリース
中の異物や増稠剤粒子の影響が挙げられるが、近年、問
題となっているのは潤滑グリースに起因する騒音である
。すなわち、軸受の転動体と転走面の間の微小すき間に
侵入した潤滑グリース中の異物や増稠剤粒子がくだけた
り、つぶれたりする時に軸受を振動させ、それが軸受の
騒音として現われる。The noise generated from this bearing, together with the noise generated from other parts, raises the overall noise level of the device. Causes of this bearing noise include problems with bearing machining and assembly accuracy, mounting accuracy, and the effects of foreign matter and thickener particles in the grease used as a lubricant, but in recent years, this has become a problem. is the noise caused by lubricating grease. In other words, when foreign matter or thickener particles in the lubricating grease that have entered the tiny gap between the rolling elements and the raceway of the bearing break or collapse, they cause the bearing to vibrate, which manifests itself as bearing noise.
低騒音を要求される軸受には、異物混入防止のため厳密
に管理された製造工程により製造されるリチウム石鹸グ
リースが広く用いられているが、近年の使用条件の過酷
化により高温でも長期間安定な性能を発揮するグリース
が求められるようになってきた。Lithium soap grease, which is manufactured through a strictly controlled manufacturing process to prevent foreign matter from entering, is widely used in bearings that require low noise, but due to harsher usage conditions in recent years, it is not stable for long periods of time even at high temperatures. There is a growing demand for grease that exhibits excellent performance.
この様な要求に対して、リチウム石鹸グリースに比へて
高温でも安定なゲル構造を有するウレアグリースを用い
ようという試みがなされているが、ウレアグリースはそ
の増稠剤粒子の性質上、軸受騒音を発生させやすく、低
騒音を要求される軸受にはほとんど普及していない。In response to these demands, attempts have been made to use urea grease, which has a gel structure that is more stable at high temperatures than lithium soap grease, but urea grease has problems with bearing noise due to the nature of its thickener particles. It is not widely used in bearings that require low noise.
本発明者らは、まずウレアグリースによる軸受騒音発生
の原因を究明するため市販ウレアグリースに関して分析
した結果、グリース中のウレア化合物の単位粒子(また
は単位繊維、以下口)の長径(または繊維長さ)は、太
きくても1104L程度でほとんどが5ヰ■以下である
にもかかわらず、その単位粒子が集まった20〜200
4m程度の凝集体が多数存在し、この凝集体が軸受騒音
の原因である事を突きとめた。The present inventors first analyzed commercially available urea grease in order to investigate the cause of bearing noise caused by urea grease. ) is about 1104L at most, and most of them are less than 5ヰ■, but the unit particles are 20 to 200
There were many aggregates of about 4 m in length, and it was determined that these aggregates were the cause of the bearing noise.
また、下記に示すアミン類、ジイソシアネート類、基油
各々の組合せについて、アミンとジイソシアネートの反
応により生成するウレア化合物と基油の重量比が10対
90になるような配合を作成し、アミンの基油溶液とジ
インシアネートの基油溶液を混合して反応させ、170
℃まで加熱攪拌処理を行ない、室温まで放冷後、三木ロ
ールミルで仕上げ処理するという一般的な製法により試
作して分析を行なった。In addition, for each of the combinations of amines, diisocyanates, and base oils shown below, a formulation was created such that the weight ratio of the urea compound produced by the reaction of the amine and diisocyanate to the base oil was 10:90, and the amine group The oil solution and the diincyanate base oil solution are mixed and reacted, and 170
A prototype was prepared and analyzed using a common method of heating and stirring to ℃, cooling to room temperature, and finishing with a Miki roll mill.
アミン類
n−プロピルアミン、 イソプロピルアミンn−ブチル
アミン イソブチルアミンS−ブチルアミン
n−ペンチルアミン3−メチルブチルアミン、n−へブ
チルアミンn−オクチルアミン、 2−エチルヘキシル
アミンn−ドデシルアミン、 n−テトラデシルアミン
n−ヘキサデシルアミン、n−オクタデジルアミンアニ
リン 4−ビフェニルアミンp−フェネチジ
ン 、 p−7ニシジンp−ドデシルアニリン、シクロ
ペンチルアミンシクロヘキシルアミン。Amines n-propylamine, isopropylamine n-butylamine isobutylamine S-butylamine
n-pentylamine 3-methylbutylamine, n-hebutylamine n-octylamine, 2-ethylhexylamine n-dodecylamine, n-tetradecylamine n-hexadecylamine, n-octadecylamine aniline 4-biphenylamine p- Phenetidine, p-7 nisidine p-dodecylaniline, cyclopentylamine cyclohexylamine.
ジヒドロアビエチルアミン。Dihydroabiethylamine.
3.5.5− )リメチルヘキシルアミン。3.5.5-) Limethylhexylamine.
オレイルアミン
ジインシアネート類
1.5−ナフチレンジイソシアネート
4.4′−ジフェニルメタンジイソシアネート2.4−
トリレンジイソシアネート3.3′−ジメチル−4
,4′−ビフェニレンジインシアネート
ヘキサメチレンジイソシアネート
基 油
α−オレフィンオリゴマー(40℃動粘度30cSt)
パラフィン系鉱油 00℃動粘度67cSt)ジ
メチルシリコーン (25℃動粘度200cSt)ペ
ンタエリスリトールテトラエステル
(40℃動粘度31cSt)
分析結果は、オレイルアミンと3.3′−ジメチル−4
,4′−ビフェニレンジイソシアネートを基油中で反応
させたグリースを除く、全ての試作グリースにおいて2
0〜200.鵬程度の凝集体が多数存在する事を確認し
た。Oleylamine diisocyanates 1.5-Naphthylene diisocyanate 4.4'-Diphenylmethane diisocyanate 2.4-
Tolylene diisocyanate 3.3'-dimethyl-4
, 4'-biphenylene diisocyanate hexamethylene diisocyanate base oil α-olefin oligomer (40°C kinematic viscosity 30 cSt)
Paraffinic mineral oil (Kinematic viscosity at 00°C, 67 cSt) Dimethyl silicone (Kinematic viscosity at 25°C, 200 cSt) Pentaerythritol tetraester (Kinematic viscosity at 40°C, 31 cSt) Analysis results show that oleylamine and 3.3'-dimethyl-4
, 2 in all prototype greases except for the grease in which 4'-biphenylene diisocyanate was reacted in the base oil.
0-200. It was confirmed that there were many aggregates of Peng size.
20〜200川■程度の凝集体の存在する試料のうち、
n−オクチルアミンと4,4′−ジフェニルメタンジイ
ソシアネートをパラフィン系鉱油(40℃動粘度67c
St)中で反応させたグリース、シクロヘキシルアミン
と4,4′−ジフェニルメタンジイソシアネートをペン
タエリスリトールテトラエステル(40℃動粘度31c
St)中で反応させたグリースについて、さらに3本ロ
ールミルを通過させる処理を試みた結果、20回通過さ
せると約50%程度減る事が確認された。しかし、さら
に100回通過させても若干の減少は認められるが完全
に消失するわけではなく、また、この様な方法は過大な
時間と労力を要し、実用には供し難い、他の仕上げ処理
方法としてホモジナイザー処理、ボールミル処理、コロ
イドミル処理を試みたが、顕著な効果は得られなかった
0以上の様に、−旦凝集体ができてしまうと、機械的処
理では限界があると考えられた。Among the samples containing about 20 to 200 aggregates,
n-octylamine and 4,4'-diphenylmethane diisocyanate were dissolved in paraffinic mineral oil (40°C kinematic viscosity 67c).
Grease, cyclohexylamine and 4,4'-diphenylmethane diisocyanate reacted in pentaerythritol tetraester (40℃ kinematic viscosity 31c
As a result of trying to further pass the grease reacted in St) through a three-roll mill, it was confirmed that the grease was reduced by about 50% after passing through it 20 times. However, even after 100 passes, a slight decrease is observed, but it does not disappear completely. In addition, such a method requires excessive time and labor, and is difficult to use in practical use. Homogenizer treatment, ball mill treatment, and colloid mill treatment were tried as methods, but no significant effects were obtained.As mentioned above, it is thought that once aggregates are formed, there is a limit to mechanical treatment. Ta.
凝集体の存在しなかったオレイルアミンと3.3′−ジ
メチル−4,4′−ビフェニレンジインシアネートを基
油中で反応させたグリースは、優れた低騒音性能を有し
ているが、長期間静置保存すると、たとえば、鉱油を基
油とするグリース(増稠剤含有量20重量%)では、8
0日間で混和稠度(JIS K 22205.3)が2
71から328に変化するというように、かなり軟化す
る傾向を示し、また滴点試験(JIS K 22205
.4)では180℃以下で滴下してしまい、現実的には
150℃以下の温度でしか使用できない、すなわち、こ
の増稠剤を使用したグリースは、他のウレアグリースと
比較して貯蔵安定性および高温安定性が劣るという問題
点があった。Grease made by reacting oleylamine with no aggregates and 3,3'-dimethyl-4,4'-biphenylene diinocyanate in base oil has excellent low noise performance, but does not remain quiet for a long time. For example, grease based on mineral oil (thickener content: 20% by weight) has a
The mixing consistency (JIS K 22205.3) was 2 in 0 days.
71 to 328, showing a tendency to soften considerably, and dropping point test (JIS K 22205
.. In 4), it drips at temperatures below 180°C, and in reality it can only be used at temperatures below 150°C.In other words, greases using this thickener have poor storage stability and stability compared to other urea greases. There was a problem that high temperature stability was poor.
[問題を解決するための手段]
そこで、本発明者らは、オレイルアミンと3.3′−ジ
メチル−4,4′−ビフェニレンジイソシアネートを基
油中で反応させたグリースの優れた低騒音性能を損なう
事なく、優れた貯蔵安定性および高温安定性を有するよ
うに、その増稠剤について鋭意研究を重ねた結果、以下
の一般式で示される増稠剤を見いだした。[Means for Solving the Problem] Therefore, the present inventors have proposed a method that impairs the excellent low-noise performance of a grease prepared by reacting oleylamine and 3,3'-dimethyl-4,4'-biphenylene diisocyanate in a base oil. As a result of extensive research into thickeners that have excellent storage stability and high-temperature stability, we have discovered a thickener represented by the following general formula.
一般式
%式%
[式中、R1およびR3は炭素数8〜18のアルキル基
とオレイル基の混合体であり、且つオレイル基の割合が
5〜95モル%である。またR2は3,3′−ジメチル
−4,4′−ビフェニレン基を表わす、]この式で、R
1およびR3に炭素数が7以下のアルキル基やフェニル
基、シクロアルキル基を含む場合は、増稠剤の凝集体が
生成し本発明には適さない。R1およびR3に炭素数1
8を超えるアルキル基を含む場合は、その原料となる長
鎖のモノアミンを経済的価格で入手する事が難しいので
実用には適さない、また、R1およびR3中に占めるオ
レイル基の割合は、5〜95モル%好ましくは20〜7
0モル%であり、5モル%未満では増稠剤の凝集体が生
威し、95モル%を越えると貯蔵安定性および高温安定
性が劣るので、ともに本発明には適さない。General Formula % Formula % [In the formula, R1 and R3 are a mixture of an alkyl group having 8 to 18 carbon atoms and an oleyl group, and the proportion of the oleyl group is 5 to 95 mol%. In addition, R2 represents a 3,3'-dimethyl-4,4'-biphenylene group.] In this formula, R
If 1 and R3 contain an alkyl group, a phenyl group, or a cycloalkyl group having 7 or less carbon atoms, aggregates of the thickener will be formed, which is not suitable for the present invention. 1 carbon number in R1 and R3
If it contains more than 8 alkyl groups, it is difficult to obtain a long-chain monoamine as a raw material at an economical price, so it is not suitable for practical use.In addition, the proportion of oleyl groups in R1 and R3 is ~95 mol% preferably 20-7
If it is less than 5 mol%, aggregates of the thickener will grow, and if it exceeds 95 mol%, storage stability and high temperature stability will be poor, and both are not suitable for the present invention.
すなわち、上記一般式で示される増稠剤と基油からなる
ウレアグリース組成物は、優れた低騒音性能を有し、か
つ、60日間静置保存での混和稠度の変化が±lO以下
という貯蔵安定性および滴点が190℃以上という高温
安定性を有する。That is, the urea grease composition consisting of the thickener and base oil represented by the above general formula has excellent low noise performance and can be stored for 60 days with a change in mixing consistency of ±1O or less. It has stability and high temperature stability with a dropping point of 190°C or higher.
さらに研究を重ねた結果、上記一般式のR1およびR3
に含まれるアルキル基が異なる2種類以上のグリースを
別々に製造し、それらを混合する事により、満点が混合
前のいずれのグリースよりも高くなり、さらに高温でも
安定なゲル構造を有するグリースが得られる事を見いだ
した。グリースの混合比としては、混合された2種類の
グリースの増稠剤の重量比が1対S9になるような混合
比でも滴点の上昇は認められるが、250℃以上の満点
を有するグリースを得るには、異なる増稠剤の重量比が
10〜90対90〜10になるような混合比が望ましい
。As a result of further research, R1 and R3 of the above general formula
By separately manufacturing two or more types of grease with different alkyl groups and mixing them, a grease with a higher perfect score than any of the greases before mixing and a gel structure that is stable even at high temperatures can be obtained. I found something that can be done. As for the mixing ratio of the two types of grease, an increase in the dropping point is observed even when the weight ratio of the thickener of the two types of grease is 1:S9. In order to achieve this, a mixing ratio such that the weight ratio of different thickeners is 10-90 to 90-10 is desirable.
以上のような方法によりウレアグリースの特徴である高
温安定性を有し、かつ、リチウム石鹸グリースより優れ
た低騒音性能を有するきわめて有用なウレアグリースの
完成に至った。By the method described above, we have completed an extremely useful urea grease that has the high temperature stability characteristic of urea grease and also has lower noise performance that is superior to lithium soap grease.
本発明の特許請求の範囲第1項記載のウレアグリースは
、たとえば、全アミン、全ジイソシアネートそれぞれの
基油溶液を、80−120℃で混合し、攪拌しながら毎
分1〜5℃の速度で170〜200℃まで昇温させ、放
冷後、3本ロールミルで仕上げ処理するというような、
公知の一般的な製法により得ることができる。また、本
発明の特許請求の範囲第2項記載の増稠剤中に異なるア
ルキル基を含む2種類以上のグリースの混合も、それら
グリースが均一によく混じり有ってさえいれば、その方
法、装置は特に限定されない、ただし、本発明の高温に
おいても安定なゲル構造を有する特許請求の範囲第2項
記載のグリースを得るためには、グリース同士を混合す
る必要があり。The urea grease described in claim 1 of the present invention can be produced by mixing base oil solutions of all amines and all diisocyanates at 80 to 120°C, and mixing them at a rate of 1 to 5°C per minute while stirring. The temperature is raised to 170-200℃, left to cool, and then finished with a three-roll mill.
It can be obtained by a known general manufacturing method. Furthermore, the method for mixing two or more types of greases containing different alkyl groups in their thickeners as set forth in claim 2 of the present invention can be carried out as long as the greases are uniformly and well mixed. The apparatus is not particularly limited, but in order to obtain the grease of the present invention having a stable gel structure even at high temperatures, it is necessary to mix the greases.
ジインシアネートとアミンの反応時に異なる2種類以上
のアルキルアミンを混合しても、目的とするウレアグリ
ースは得られない。Even if two or more different types of alkylamines are mixed during the reaction of diincyanate and amine, the desired urea grease cannot be obtained.
本発明に用いる基油は一般に知られている潤滑油であり
、鉱油、α−オレフィンオリゴマー シリコーン油、ジ
エステル油、トリエステル油、テトラエステル油、フッ
素油、リン酸エステル油、ヒマシ油、フェニルエーテル
油、アルキルナフタレン、アルキレングリコール等でア
ル。The base oils used in the present invention are generally known lubricating oils, such as mineral oil, α-olefin oligomer silicone oil, diester oil, triester oil, tetraester oil, fluorine oil, phosphate ester oil, castor oil, and phenyl ether oil. Al with oil, alkylnaphthalene, alkylene glycol, etc.
本発明のジウレアグリース組成物において、増稠剤であ
るジウレア化合物の含有量は2〜40重量%、好ましく
は5〜35重量%である。ジウレア化合物の含有量が2
重量%未渦の場合には、増稠効果が少なくグリース状に
はならず、また、40重量%を越えるとグリースは硬く
なりすぎて十分な潤滑効果が得られない。In the diurea grease composition of the present invention, the content of the diurea compound as a thickener is 2 to 40% by weight, preferably 5 to 35% by weight. Diurea compound content is 2
When the weight percent is not swirled, the thickening effect is small and the grease does not form.If it exceeds 40 weight percent, the grease becomes too hard and a sufficient lubricating effect cannot be obtained.
本発明のジウレアグリースには、その目的とする性質を
損ねることなしに、さらにその性能を向上させるため本
来の成分とは別に、酸化防止剤、防錆剤、極圧剤など各
種添加剤を加える事ができる。In addition to the original ingredients, various additives such as antioxidants, rust preventives, and extreme pressure agents are added to the diurea grease of the present invention in order to further improve its performance without impairing its intended properties. I can do things.
[作用]
本発明の作用は概ね以下のように考えられるが、詳細な
メカニズムを解明するには至っていない。[Effect] The effect of the present invention is generally considered to be as follows, but the detailed mechanism has not yet been elucidated.
本発明のジウレアグリースは、第1に、その増稠剤中に
オレイル基と炭素数8〜18のアルキル基とを適度に混
在させる事を特徴とする。この方法によりオレイルアミ
ンと3,3′−ジメチル−4,4′−ビフエニレンジイ
ソシアネートを基油中で反応させて得られたグリースの
貯蔵安定性および高温安定性が改良された。これは、炭
化水素基が二重結合に対して同じ側にあるシス構造をと
り、炭素鎖の中央部分で大きく折れ曲った立体構造を有
するオレイル基、すなわちシス−8−オクタデセニル基
がジウレア分子中に存在するため、その立体構造の影響
で増稠剤粒子の凝集体ができにくいが、その立体構造ゆ
えの増稠剤としての不安定さを適度のアルキル基の混合
で緩和したものと考えられる。The diurea grease of the present invention is first characterized in that an oleyl group and an alkyl group having 8 to 18 carbon atoms are appropriately mixed in the thickener. This method improved the storage stability and high temperature stability of a grease obtained by reacting oleylamine and 3,3'-dimethyl-4,4'-biphenylene diisocyanate in a base oil. This has a cis structure in which the hydrocarbon group is on the same side as the double bond, and the oleyl group, or cis-8-octadecenyl group, has a largely bent three-dimensional structure in the center of the carbon chain in the diurea molecule. Because of its 3D structure, it is difficult to form thickener particle aggregates, but it is thought that the instability as a thickener due to its 3D structure was alleviated by mixing an appropriate amount of alkyl groups. .
さらに、前記方法で得られたグリースのうち増稠剤に異
なるアルキル基を含む2種類以上のグリースを混合する
事が第2の特徴である。この混合により高温安定性がさ
らに改良された。このように混合する事によって滴点が
高くなる理由は、異なる性質を有する粒子、すなわち増
稠剤中のアルキル基の異なる粒子が相互にゲル構造を補
強し合うためと考えられる。Furthermore, the second feature is that two or more types of greases containing different alkyl groups as thickeners are mixed among the greases obtained by the above method. This blend further improved high temperature stability. The reason why the dropping point increases by mixing in this way is thought to be that particles with different properties, ie, particles with different alkyl groups in the thickener, mutually reinforce the gel structure.
一般に、ジインシアネート溶液に2種類以上のモノアミ
ンを均一に分散させた溶液を加え反応させると、その両
端に結合しているアミン残基の違いによって3種類以上
のジウレア化合物が生成し、それらの生成割合は使用す
るモノアミンの反応性と混合比による。しかし、それら
ジウレア化合物分子はグリース中で、それぞれの種類毎
に別々の粒子を作っているわけではなく、複雑に混じり
合い、厳密には個々の粒子は少しずつ異なる事はあって
も、類似した性質を有する粒子になっていると考えられ
る。従って、ジイソシアネートとモノアミンの反応時に
異なる2種類以上のアルキルアミンを混合しても、異な
る性質を有する増稠剤粒子が相互にゲル構造を補強し合
う事はでき得す、高滴点を有する本発明の特許請求の範
囲第2項記載のジウレアグリースは得られない。Generally, when a solution in which two or more types of monoamines are uniformly dispersed is added to a diincyanate solution and reacted, three or more types of diurea compounds are generated depending on the difference in the amine residues bonded to both ends. The proportion depends on the reactivity of the monoamine used and the mixing ratio. However, these diurea compound molecules do not form separate particles for each type in grease, but are mixed together in a complex manner, and although the individual particles may differ slightly from each other, they are similar. It is thought that the particles have certain properties. Therefore, even if two or more different types of alkylamines are mixed during the reaction of diisocyanate and monoamine, thickener particles with different properties can mutually reinforce the gel structure. The diurea grease described in claim 2 of the invention cannot be obtained.
[実施例]
本発明を以下の実施例、比較例により具体的に説明する
。ここで実施例、比較例に用いる略語、用語、試験方法
は以下の通りである。[Example] The present invention will be specifically explained by the following Examples and Comparative Examples. The abbreviations, terms, and test methods used in Examples and Comparative Examples are as follows.
■TO[] I
3.3 −ジメチル−4,4′−ビフェニレンジインシ
アネート
■鉱油
パラフィン系精製鉱油 40℃動粘度87cSt■α−
オレフィン
α−オレフィンオリゴマー 40℃動粘度30cSt■
フェニルエーテル
アルキルジフェニルエーテル40℃動粘に87cSt■
オレイル/非オレイル比
グリース中の全ジウレア化合物の両末端基のオレイル基
とそれ以外の炭化水素基(非オレイル基)とのモル比を
示す、たとえば、オレイル基が30モル%、非オレイル
基が10モル%ならば、90/ 10と表示する。■TO[] I 3.3-dimethyl-4,4'-biphenylene diinocyanate ■Mineral oil Paraffin-based refined mineral oil 40°C kinematic viscosity 87 cSt ■α-
Olefin α-olefin oligomer 40℃ kinematic viscosity 30cSt■
Phenyl ether alkyl diphenyl ether Kinematic viscosity at 40℃ 87cSt■
Oleyl/non-oleyl ratio Indicates the molar ratio between the oleyl groups and other hydrocarbon groups (non-oleyl groups) of both terminal groups of all diurea compounds in the grease. For example, oleyl group is 30 mol%, non-oleyl group is If it is 10 mol%, it is expressed as 90/10.
■混和稠度 JIS K 22205.3による。■Mixing consistency According to JIS K 22205.3.
■満点 JIS K 22205.4による。■Full score According to JIS K 22205.4.
■貯蔵安定度
グリース約500gを、25±3℃で60日間、容器に
密閉保存した後の混和稠度を測定し、下式で試験前との
積度差を算出する。■Storage Stability Approximately 500 g of grease is stored in a sealed container at 25±3°C for 60 days, then the mixing consistency is measured, and the difference in consistency from before the test is calculated using the following formula.
稠度差=60日後の混和稠度−試験前の混和稠度■凝集
体の個数
きょう雑物試験(JIS K 22205.9)を応用
し、スライドガラスにグリースを塗在し、カバーガラス
をかぶせてグリース膜厚を30pmにし、光学m微鏡(
倍率100倍)で観察し、0.46mwX0.64mm
の枠内にある20ル曽以上の大きさの凝集体を数える。Difference in consistency = Mixing consistency after 60 days - Mixing consistency before the test ■ Number of aggregates Applying the dirt test (JIS K 22205.9), apply grease to a slide glass, cover it with a cover glass, and create a grease film. The thickness was set to 30 pm, and an optical m-microscope (
Observed at 100x magnification), 0.46mw x 0.64mm
Count the aggregates with a size of 20 L or more within the frame.
・1のアンゾロン値
アンゾロンメーターはころがり軸受の振動測定器として
広く使用されており、軸受の内輪を回転させ、スラスト
荷重を負荷した外輪の振動をアンゾロンという単位で指
示する装置である0本発明では軸受6200、グリース
充てん量0.30g 、軸受内輪回転数180Or、p
、m 、スラスト荷重2.0kgという条件で、1分間
軸受を回転させ、1分後の旧ghBand(1800”
100OOH2)における指示値をアンゾロン値とし
て読み取る。・Anzolone value of 1 Anzolone meter is widely used as a vibration measuring device for rolling bearings, and is a device that rotates the inner ring of the bearing and indicates the vibration of the outer ring that is loaded with a thrust load in units of anzolone.0 This invention So, bearing 6200, grease filling amount 0.30g, bearing inner ring rotation speed 180Or, p
, m, the bearing was rotated for 1 minute under the condition of thrust load 2.0 kg, and after 1 minute the old ghBand (1800"
100OOH2) is read as the anzolone value.
表に、実施例、比較例の各グリースの配合および試験結
果を示す、各グリースの製法は次の通りである。The table shows the formulation and test results of each grease of Examples and Comparative Examples. The manufacturing method of each grease is as follows.
実施例1〜12)比較例1〜6
表に示す配合で、基油局量に全ジイソシアネートを80
℃で加熱溶解した溶液と残りの基油に全アミンを80℃
で加熱溶解した溶液を混合して20分間よく攪拌した。Examples 1 to 12) Comparative Examples 1 to 6 With the formulation shown in the table, 80% total diisocyanate was added to the base oil topical amount.
Add all amines to the solution heated and dissolved at 80°C and the remaining base oil.
The heated and dissolved solution was mixed and stirred well for 20 minutes.
この混合物を攪拌しながら平均毎分2℃の速度で190
℃まで昇温させた。室温付近まで放冷後、3本ロールミ
ルを2回通過させて、それぞれのグリースを得た。The mixture was stirred at an average rate of 2°C per minute at 190°C.
The temperature was raised to ℃. After cooling to around room temperature, each grease was passed through a three-roll mill twice to obtain each grease.
実施例13〜15
実施例2および実施例8で得たグリースを、表に示す配
合で混合し、3本ロールミルを2回通過させて、それぞ
れのグリースを得た。Examples 13 to 15 The greases obtained in Example 2 and Example 8 were mixed in the formulation shown in the table and passed through a three-roll mill twice to obtain each grease.
実施例16
実施例2)実施例6および実施例8で得たグリースを、
それぞれ重量比40対30対30で混合し、3本ロール
ミルを2回通過させて、グリースを得た。Example 16 Example 2) The grease obtained in Example 6 and Example 8 was
They were mixed at a weight ratio of 40:30:30, respectively, and passed through a three-roll mill twice to obtain a grease.
比較例7〜IO
市販ウレアグリースおよび市販低騒音リチウム石鹸グリ
ースである。Comparative Examples 7 to IO A commercially available urea grease and a commercially available low-noise lithium soap grease.
実施例1〜12から、増稠剤中にオレイル基と炭素数8
〜18のアルキル基とを適度に混在させる事により、比
較例1のグリースの低騒音性能を損なう事なしに、その
貯蔵安定性および高温安定性が改良された事がわかる。From Examples 1 to 12, it is clear that the thickener contains an oleyl group and a carbon number of 8.
It can be seen that the storage stability and high-temperature stability of the grease of Comparative Example 1 were improved without impairing the low-noise performance of the grease of Comparative Example 1 by appropriately mixing the alkyl groups of 1 to 18.
実施例1〜12のグリースは、滴屯は市販低騒音リチウ
ム石鹸グリースと同程度であるが、20枇1以りの凝集
体は全く存在せず、また、アンゾロン値が11.5〜1
3,5であり、比較例7〜10に示す市販ウレアグリー
スおよび市販低騒音リチウム石鹸グリースよりも優れた
低騒音性能を有している事は明らかである。The greases of Examples 1 to 12 had the same level of drop density as commercially available low-noise lithium soap greases, but there were no aggregates larger than 20 mm, and the anzolone value was 11.5 to 1.
3.5, and it is clear that it has superior low-noise performance to the commercially available urea greases and commercially available low-noise lithium soap greases shown in Comparative Examples 7 to 10.
実施例11および実施例12のグリースは、増稠剤中に
異なるアルキル基を有するが、ジイソシアネートとの反
応時に異なる2種類のアルキルアミンを加えたもので、
グリース同士を混合したものではないため高滴点を有し
ない。The greases of Example 11 and Example 12 have different alkyl groups in the thickener, but two different types of alkyl amines were added during the reaction with the diisocyanate.
Since it is not a mixture of greases, it does not have a high dropping point.
実施例13〜16は、増稠剤に異なるアルキル基を有す
る本発明の特許請求の範囲第1項記載のグリースを2種
類以上混合したものであり、いずれのグリースも満点の
上昇が認められる。特に実施例14〜16は、ウレアグ
リースの特徴である優れた高温安定性と市販低騒音リチ
ウム石鹸グリースよりも優れた低騒音性能を有する極め
て有用なグリースである。Examples 13 to 16 are mixtures of two or more types of greases according to claim 1 of the present invention having different alkyl groups in their thickeners, and all of the greases were recognized to have a perfect score. In particular, Examples 14 to 16 are extremely useful greases that have excellent high-temperature stability, which is a characteristic of urea greases, and low-noise performance that is superior to commercially available low-noise lithium soap greases.
比較例1のグリースは、優れた低騒音性能を有するが、
適度なアルキル基の混在がないため高温安定性と貯蔵安
定性が本発明グリースより劣っている。The grease of Comparative Example 1 has excellent low noise performance, but
Since there is no appropriate amount of alkyl groups, the high temperature stability and storage stability are inferior to the grease of the present invention.
比較例2〜5のグリースは、その増稠剤中に炭素数7以
下のアルキル基またはシクロアル午ル基またはフェニル
基を含むので、増稠剤の凝集体が生成し、目的とする低
騒音性能を有していない。Since the greases of Comparative Examples 2 to 5 contain an alkyl group having 7 or less carbon atoms, a cycloalkyl group, or a phenyl group in the thickener, aggregates of the thickener are formed and the desired low noise performance is not achieved. does not have.
比較例6は増稠剤中のオレイル基が5モル%未満である
ため、増稠剤の凝集体が生威し、目的とする低騒音性能
を有していない。In Comparative Example 6, since the oleyl group in the thickener was less than 5 mol %, aggregates of the thickener were present and the desired low noise performance was not achieved.
(発明の効果〕
本発明に係る低騒音ウレアグリース組成物は、その増稠
剤であるジウレア化合物粒子の20iL口以上の凝集体
の存在しない微細なジウレア化合物結晶の分散系であり
、しかも従来と同様の集注により製造することが可能で
ある。(Effects of the Invention) The low-noise urea grease composition according to the present invention is a dispersion system of fine diurea compound crystals free of aggregates of 20 iL or more of diurea compound particles as a thickener, and is different from the conventional one. It is possible to manufacture by a similar concentrating method.
得られたジウレアグリース組成物は、市販低騒芹リチウ
ム石鹸グリースに優る低騒音性能および高温安定性を有
する事が確認された。The obtained diurea grease composition was confirmed to have low noise performance and high temperature stability superior to commercially available low noise lithium soap greases.
すなわち、本発明は従来の低騒音リチウム石鹸グリース
より耐熱性、耐久性の優れた低騒音ウレアグリースを提
供できるという効果を有する。That is, the present invention has the effect of providing a low-noise urea grease that has better heat resistance and durability than conventional low-noise lithium soap grease.
Claims (2)
、R1およびR3は炭素数8〜18のアルキル基とオレ
イル基の混合体であり、且つオレイル基の割合が5〜9
5モル%である、またR2は3,3′−ジメチル−4,
4′−ビフェニレン基を表わす。]で示されるウレア化
合物2〜40重量%と基油98〜60重量%からなるこ
とを特徴とする低騒音ウレアグリース組成物。(1) General formula R1-NHCONH-R2-NHCONH-R3 [wherein R1 and R3 are a mixture of an alkyl group having 8 to 18 carbon atoms and an oleyl group, and the ratio of oleyl groups is 5 to 9
5 mol%, and R2 is 3,3'-dimethyl-4,
Represents a 4'-biphenylene group. A low-noise urea grease composition comprising 2 to 40% by weight of a urea compound represented by the following formula and 98 to 60% by weight of a base oil.
種類以上の混合体であって、高温においても安定なグリ
ース構造を保つことを特徴とする低騒音ウレアグリース
組成物。(2) 2 of the grease composition according to claim 1
A low-noise urea grease composition that is a mixture of more than one type and maintains a stable grease structure even at high temperatures.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3961290A JPH03243696A (en) | 1990-02-22 | 1990-02-22 | Low-noise urea grease composition |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP3961290A JPH03243696A (en) | 1990-02-22 | 1990-02-22 | Low-noise urea grease composition |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH03243696A true JPH03243696A (en) | 1991-10-30 |
Family
ID=12557933
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP3961290A Pending JPH03243696A (en) | 1990-02-22 | 1990-02-22 | Low-noise urea grease composition |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH03243696A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004053032A1 (en) * | 2002-12-10 | 2004-06-24 | Shell Internationale Research Maatschappij B.V. | Urea grease composition |
JP2008074978A (en) * | 2006-09-21 | 2008-04-03 | Showa Shell Sekiyu Kk | Urea grease composition |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5951998A (en) * | 1982-09-17 | 1984-03-26 | Chuo Yuka Kk | Triurea grease composition |
JPS60231796A (en) * | 1984-05-02 | 1985-11-18 | Showa Shell Sekiyu Kk | Urea grease composition |
JPS62250097A (en) * | 1986-04-22 | 1987-10-30 | Nippon Oil Co Ltd | Diurea grease composition |
JPH01284591A (en) * | 1988-05-12 | 1989-11-15 | Kyodo Yushi Kk | Urea grease composition |
JPH0277494A (en) * | 1988-09-14 | 1990-03-16 | Showa Shell Sekiyu Kk | Urea grease composition improved in acoustic performance |
-
1990
- 1990-02-22 JP JP3961290A patent/JPH03243696A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS5951998A (en) * | 1982-09-17 | 1984-03-26 | Chuo Yuka Kk | Triurea grease composition |
JPS60231796A (en) * | 1984-05-02 | 1985-11-18 | Showa Shell Sekiyu Kk | Urea grease composition |
JPS62250097A (en) * | 1986-04-22 | 1987-10-30 | Nippon Oil Co Ltd | Diurea grease composition |
JPH01284591A (en) * | 1988-05-12 | 1989-11-15 | Kyodo Yushi Kk | Urea grease composition |
JPH0277494A (en) * | 1988-09-14 | 1990-03-16 | Showa Shell Sekiyu Kk | Urea grease composition improved in acoustic performance |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2004053032A1 (en) * | 2002-12-10 | 2004-06-24 | Shell Internationale Research Maatschappij B.V. | Urea grease composition |
AU2003299220B2 (en) * | 2002-12-10 | 2007-03-22 | Shell Internationale Research Maatschappij B.V. | Urea grease composition |
JP2008074978A (en) * | 2006-09-21 | 2008-04-03 | Showa Shell Sekiyu Kk | Urea grease composition |
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