CN109054965B - Low-noise composite lithium-based grease - Google Patents

Low-noise composite lithium-based grease Download PDF

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Publication number
CN109054965B
CN109054965B CN201810761683.0A CN201810761683A CN109054965B CN 109054965 B CN109054965 B CN 109054965B CN 201810761683 A CN201810761683 A CN 201810761683A CN 109054965 B CN109054965 B CN 109054965B
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lithium
grease
oil
low
stearate soap
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CN109054965A (en
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黄学宏
陈仕棋
吕文菁
岡村征二
游淑婷
卢小蓉
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Fujian Universal Grease Co ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C10M169/06Mixtures of thickeners and additives
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M177/00Special methods of preparation of lubricating compositions; Chemical modification by after-treatment of components or of the whole of a lubricating composition, not covered by other classes
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/087Boron oxides, acids or salts
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/126Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
    • C10M2207/1265Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic used as thickening agent
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2207/00Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
    • C10M2207/10Carboxylix acids; Neutral salts thereof
    • C10M2207/12Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
    • C10M2207/125Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
    • C10M2207/128Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof
    • C10M2207/1285Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids containing hydroxy groups; Ethers thereof used as thickening agents
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/08Resistance to extreme temperature
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/76Reduction of noise, shudder, or vibrations
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00Specified use or application for which the lubricating composition is intended
    • C10N2040/02Bearings

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The invention relates to lubricating grease, in particular to low-noise composite lithium base grease. The low-noise composite lithium-based grease comprises the following raw materials in parts by mass: lithium stearate soap and 12-hydroxystearic acid lithium soap: 13% -15%, base oil (ester oil/ether oil): 70-80%, antioxidant: 1% -5%, antirust agent: 1% -5%, boric acid alcohol solution: 0.5% -3%. The lithium grease disclosed by the invention is excellent in high-temperature performance and good in low-noise performance by adding the boric acid alcohol solution, and the service life of the lithium grease disclosed by the invention is 2-4 times that of the lithium grease at 165 ℃; the bearing is suitable for the motor bearing with low noise performance in a wide temperature range.

Description

Low-noise composite lithium-based grease
Technical Field
The invention relates to lubricating grease, in particular to low-noise composite lithium base grease.
Background
At present, with the development and research of grease, the grease is mainly embodied in long service life, high/low temperature, high/low speed use, low noise and the like. The development of low-noise grease has become a popular research direction abroad, and the research reports are less at home at present. The conventional complex lithium grease has excellent high temperature performance but poor low noise performance, and on the contrary, the lithium grease has excellent low noise performance but poor high temperature resistance at a high temperature of 150 ℃ or more than 150 ℃.
Disclosure of Invention
The invention aims to provide a low-noise composite lithium-based grease. According to the invention, a special additive boric acid is added and dissolved in alcohol (60-80 ℃) to prepare a novel composite lithium base, and the composite lithium base grease with excellent low-noise performance and excellent high-temperature resistance is obtained after treatment, wherein the service life of the composite lithium base grease is 2-4 times that of a common lithium soap base.
In order to achieve the purpose, the invention adopts the following technical scheme:
the low-noise composite lithium-based grease comprises the following raw materials in parts by mass:
lithium stearate soap with 12 hydroxy stearate soap: 13% -15%;
base oil: 70% -80%;
antioxidant: 1% -5%;
antirust agent: 1% -5%;
boric acid alcohol solution: 0.5% -3%.
Wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 1: 4.
The base oil is one or more of ester oil, ether oil, mineral oil and synthetic hydrocarbon oil.
Wherein the antioxidant is one or more of octyl diphenylamine, butyl diphenylamine, diisooctyl diphenylamine, phenolic ester and alkyl phenylamine.
Wherein the antirust agent is one or more of calcium petroleum sulfonate, barium petroleum sulfonate and span 80.
Wherein the mass fraction of boric acid in the boric acid alcohol solution is 0.5-3%.
The method for compounding the lithium base grease with low noise comprises the following steps:
(1) mixing lithium hydroxide with stearic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at 100-130 ℃ (wherein lithium stearate soap and 12-hydroxystearic acid soap are prepared in the process);
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding boric acid alcohol solution, antioxidant and antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
The invention has the following remarkable advantages:
(1) after the lithium-based grease is added with the boric acid alcohol solution, the high-temperature performance (dropping point) is close to that of the composite lithium-based grease, the low-noise performance is good, and the service life of the lithium-based grease is 2-4 times that of the lithium-based grease at 165 ℃;
(2) the lithium-based grease is suitable for long-life lubrication in a wide temperature range (mainly ester oil);
(3) the lithium-based grease is suitable for motor bearings with low noise performance in a wide temperature range, is applied to automobiles, and can be suitable for bearings with high-temperature long-time work and low noise performance.
Drawings
FIG. 1 is a photograph of microscopic particles of a sample of comparative example 1;
FIG. 2 is a photograph of microscopic particles of a sample of comparative example 2;
FIG. 3 is a photograph of microscopic particles of a sample of comparative example 3;
FIG. 4 is a photograph of microscopic particles of a sample of comparative example 4;
FIG. 5 is a photograph of microscopic particles of a sample of example 1;
FIG. 6 is a photograph of microscopic particles of a sample of example 2;
FIG. 7 is a photograph of microscopic particles of a sample of example 3;
FIG. 8 shows the results of the low noise test (decibel values); a, B, C, D, E, F, G in the figure are comparative example 1, comparative example 2, comparative example 3, comparative example 4, example 1, example 2 and example 3 in sequence;
FIG. 9 shows the results of the BVT bearing vibration mid-frequency test; a, B, C, D, E, F, G in the figure are comparative example 1, comparative example 2, comparative example 3, comparative example 4, example 1, example 2 and example 3 in sequence;
FIG. 10 shows the result of the BVT bearing vibration high frequency test; a, B, C, D, E, F, G in the figure are comparative example 1, comparative example 2, comparative example 3, comparative example 4, example 1, example 2 and example 3 in this order.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Example 1
The low-noise composite lithium-based grease comprises the following raw materials in parts by mass:
lithium stearate soap with 12 hydroxy stearate soap: 13 percent (wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 1: 4),
base oil (ester oil/ether oil): 77.5 percent of the total weight of the mixture,
antioxidant: 2 percent of the total weight of the mixture,
antirust agent: 4.5 percent of the total weight of the mixture,
boric acid alcohol solution: 3 percent.
The preparation method of the low-noise composite lithium-based grease comprises the following steps:
(1) mixing lithium hydroxide, stearic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at the temperature of 100-130 ℃;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding 3wt% boric acid alcohol solution, antioxidant and antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
Wherein the antioxidant is diisooctyl diphenylamine, and the antirust agent is span 80.
Example 2
The low-noise composite lithium-based grease comprises the following raw materials in parts by mass:
lithium stearate soap with 12 hydroxy stearate soap: 13 percent (wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 1: 4),
base oil (ester oil/ether oil): 79.5 percent of the total weight of the mixture,
antioxidant: 2 percent of the total weight of the mixture,
antirust agent: 4.5 percent of the total weight of the mixture,
boric acid alcohol solution: 1 percent.
The preparation method of the low-noise composite lithium-based grease comprises the following steps:
(1) mixing lithium hydroxide, stearic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at the temperature of 100-130 ℃;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding 1wt% boric acid alcohol solution, antioxidant and antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
Wherein the antioxidant is diisooctyl diphenylamine, and the antirust agent is span 80.
Example 3
The low-noise composite lithium-based grease comprises the following raw materials in parts by mass:
lithium stearate soap with 12 hydroxy stearate soap: 13 percent (wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 1: 4),
base oil (ester oil/ether oil): 80 percent of the total weight of the mixture,
antioxidant: 2 percent of the total weight of the mixture,
antirust agent: 4.5 percent of the total weight of the mixture,
boric acid alcohol solution: 0.5 percent.
The preparation method of the low-noise composite lithium-based grease comprises the following steps:
(1) mixing lithium hydroxide, stearic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at the temperature of 100-130 ℃;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding 0.5wt% of boric acid alcohol solution, an antioxidant and an antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
Wherein the antioxidant is diisooctyl diphenylamine, and the antirust agent is span 80.
Comparative example
Comparative example 1
Lithium stearate soap with 12 hydroxy stearate soap: 13 percent (wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 1: 4),
base oil (ester oil/ether oil): 80.5 percent of the total weight of the mixture,
antioxidant: 2 percent of the total weight of the mixture,
antirust agent: 4.5 percent of the total weight of the mixture,
the preparation method of the lithium grease comprises the following steps:
(1) mixing lithium hydroxide, stearic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at the temperature of 100-130 ℃;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding an antioxidant and an antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
Wherein the antioxidant is diisooctyl diphenylamine, and the antirust agent is span 80.
Comparative example 2
Lithium stearate soap/12 lithium hydroxystearate soap: 13 percent (wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 3: 7),
base oil (ester oil/ether oil): 80.5 percent of the total weight of the mixture,
antioxidant: 2 percent of the total weight of the mixture,
antirust agent: 4.5 percent of the total weight of the mixture,
the preparation method of the lithium grease comprises the following steps:
(1) mixing lithium hydroxide, stearic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at the temperature of 100-130 ℃;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding an antioxidant and an antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
Wherein the antioxidant is diisooctyl diphenylamine, and the antirust agent is span 80.
Comparative example 3
Lithium sebacate soap/12 lithium hydroxystearate soap: 13 percent (wherein the mass ratio of the lithium sebacate soap to the 12-hydroxyl lithium stearate soap is 1: 4),
base oil (ester oil/ether oil): 80.5 percent of the total weight of the mixture,
antioxidant: 2 percent of the total weight of the mixture,
antirust agent: 4.5 percent of the total weight of the mixture,
the preparation method of the composite lithium grease comprises the following steps:
(1) mixing lithium hydroxide, sebacic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at the temperature of 100-130 ℃;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding an antioxidant and an antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
Wherein the antioxidant is diisooctyl diphenylamine, and the antirust agent is span 80.
Comparative example 4
Lithium stearate soap/12 lithium hydroxystearate soap: 13 percent (wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 1: 4),
base oil (ester oil/ether oil): 77.5 percent of the total weight of the mixture,
antioxidant: 2 percent of the total weight of the mixture,
antirust agent: 4.5 percent of the total weight of the mixture,
boric acid solution: 3 percent of
The preparation method of the composite lithium grease comprises the following steps:
(1) mixing lithium hydroxide, stearic acid and 12-hydroxystearic acid with base oil, and reacting for 1 hour at the temperature of 100-130 ℃;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding 3wt% of boric acid aqueous solution antioxidant and antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
Wherein the antioxidant is diisooctyl diphenylamine, and the antirust agent is span 80.
TABLE 1 comparison of the Properties of the inventive and comparative examples
Figure DEST_PATH_IMAGE001
As can be seen from the data in Table 1, the composite lithium-based grease prepared in the embodiments 1-3 of the invention has good low-noise performance and long high-temperature resistance and service life. The low noise performance is very good as reflected in fig. 8, 9 and 10.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims (4)

1. A low-noise composite lithium-based grease is characterized in that: the raw material components comprise the following components in percentage by mass:
lithium stearate soap with 12 hydroxy stearate soap: 13% -15%;
base oil: 70% -80%;
antioxidant: 1% -5%;
antirust agent: 1% -5%;
boric acid alcohol solution: 0.5% -3%;
the sum of the mass fractions of all the raw material components is 100 percent;
wherein the mass ratio of the lithium stearate soap to the 12-hydroxyl lithium stearate soap is 1: 4;
wherein the mass fraction of boric acid in the boric acid alcohol solution is 0.5-3%;
the preparation method of the low-noise composite lithium-based grease comprises the following steps:
(1) mixing lithium hydroxide, stearic acid, 12-hydroxystearic acid and base oil, and reacting for 1 hour at the temperature of 100-130 ℃; preparing lithium stearate soap and 12-hydroxyl lithium stearate soap;
(2) continuously heating to 220-230 ℃, and stirring for 15 min;
(3) transferring to a blending kettle for cooling;
(4) adding boric acid alcohol solution, antioxidant and antirust agent;
(5) grinding for 2 times by using a three-roller mill;
(6) filtration and degassing are carried out.
2. The lithium complex base grease as claimed in claim 1, wherein: the base oil is one or more of ester oil, ether oil, mineral oil and synthetic hydrocarbon oil.
3. The lithium complex base grease as claimed in claim 1, wherein: wherein the antioxidant is one or more of octyl diphenylamine, butyl diphenylamine, diisooctyl diphenylamine, phenolic ester and alkyl phenylamine.
4. The lithium complex base grease as claimed in claim 1, wherein: wherein the antirust agent is one or more of calcium petroleum sulfonate, barium petroleum sulfonate and span 80.
CN201810761683.0A 2018-07-12 2018-07-12 Low-noise composite lithium-based grease Active CN109054965B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1083353A2 (en) * 1999-09-08 2001-03-14 Minebea Co., Ltd. Bearing having low torque, small noise and long life
CN1616612A (en) * 2003-11-13 2005-05-18 中国石油化工股份有限公司 Composite lithium base lubricant and its preparing method
CN101087868A (en) * 2004-07-30 2007-12-12 美蓓亚株式会社 Lithium grease composition sealed in a small motor bearing to reduce noise
CN102010777A (en) * 2010-12-20 2011-04-13 云南光电辅料有限公司 Grease lubricant for optical lens
CN108085096A (en) * 2017-12-25 2018-05-29 新乡市恒星科技有限责任公司 A kind of high dropping point universal lithium base grease and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1083353A2 (en) * 1999-09-08 2001-03-14 Minebea Co., Ltd. Bearing having low torque, small noise and long life
CN1616612A (en) * 2003-11-13 2005-05-18 中国石油化工股份有限公司 Composite lithium base lubricant and its preparing method
CN101087868A (en) * 2004-07-30 2007-12-12 美蓓亚株式会社 Lithium grease composition sealed in a small motor bearing to reduce noise
CN102010777A (en) * 2010-12-20 2011-04-13 云南光电辅料有限公司 Grease lubricant for optical lens
CN108085096A (en) * 2017-12-25 2018-05-29 新乡市恒星科技有限责任公司 A kind of high dropping point universal lithium base grease and preparation method thereof

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