CN109825344A - A kind of high thermal conductivity lubricating additive and preparation method thereof - Google Patents

A kind of high thermal conductivity lubricating additive and preparation method thereof Download PDF

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Publication number
CN109825344A
CN109825344A CN201910149943.3A CN201910149943A CN109825344A CN 109825344 A CN109825344 A CN 109825344A CN 201910149943 A CN201910149943 A CN 201910149943A CN 109825344 A CN109825344 A CN 109825344A
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China
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carbon nanotube
thermal conductivity
high thermal
lubricating
added
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CN201910149943.3A
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纪红兵
晏金灿
张娜
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Huizhou Research Institute of Sun Yat Sen University
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Huizhou Research Institute of Sun Yat Sen University
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Abstract

The invention discloses a kind of high thermal conductivity lubricating additives and preparation method thereof.It is made of carbon nanotube and nano silver, the quality proportioning of carbon nanotube and nano silver is respectively 5-10:1-3.The additive of carbon nanotube loaded silver can improve the dispersion performance of carbon nanotube, preferably be dispersed in lubricating grease and lubricating oil, can be used as grease additive use.The carbon nanotube loaded silver additive of preparation is high heat-conductivity conducting composite material, has excellent mechanical property and antiwear and friction reduction property.It is added in lubricating oil and lubricating grease, the thermal coefficient of lubricating oil and lubricating grease and the frictional behaviour of lubricating oil and lubricating grease can be greatly promoted.The preparation method of high thermal conductivity lubricating additive is simple to operation, and comprehensive performance is strong, and addition uses simple and convenient, has good service performance.

Description

A kind of high thermal conductivity lubricating additive and preparation method thereof
Technical field
The present invention relates to technical field of lubricant, specifically, being related to a kind of high thermal conductivity lubricating additive and its preparation side Method.
Background technique
As the improvement of the industrialization, in order to meet pursuit of the people to quality of life, the 1/3 of whole world industrial energy Because friction consumes, the 80% of the part that fails is caused by wear and tear, and heat will certainly be generated in fretting wear, Wiping contact temperature is up to 1000 DEG C.Lubricating grease plays the role of lubrication and sealing, and oil product bulk temperature is up to 60 DEG C~120 DEG C High temperature will certainly be generated when high load capacity, running at high speed, and increasingly require the lubricating action under high-temperature situation.With science and technology Fast development, the demand of the heating conduction of lubricating grease are also constantly promoted, and traditional lubricating grease is not able to satisfy some characteristics, existing Lubricating grease high temperature resistance is poor, therefore lubricating grease high thermal conductivity additive is an important research direction.
The nanocomposite of carbon nanotube loaded silver is a kind of novel lubricating additive, passes through carbon nanotube and nanometer Silver-colored is compound, had not only played the advantage of carbon nanotube high aspect ratio, but also combine Nano silver grain high heat-conductivity conducting performance, and had made up Nano silver grain disadvantage easy to reunite, add a small amount of nano silver can great advantage, the two mutual supplement with each other's advantages greatly mentions The heating conduction of carbon nanotube is risen.
Summary of the invention
It is an object of the invention to be directed to the difference of the prior art, a kind of novel high thermal conductivity lubricating additive is proposed, The heating conduction and greasy property that lubricating oil and lubricating grease can be promoted, make it have excellent comprehensive performance, can widely apply In lubricating oil and lubricating grease.
It is another object of the present invention to provide the preparation methods of above-mentioned high thermal conductivity lubricating additive.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of high thermal conductivity lubricating additive, is made of carbon nanotube and nano silver.The present invention is designed by reasonable component And optimization, probing into an optimum proportioning makes materials serve sharpest edges, is compared by many experiments, optimizes heating conduction.It is described Carbon nanotube and the quality proportioning of nano silver are respectively 5-10:1-3.The quality optimum proportioning of the carbon nanotube and nano silver point It Wei not 10:1,5:1,10:3.
The preparation method of above-mentioned high thermal conductivity lubricating additive, includes the following steps:
(1) carbon nanotube acidification is handled: carbon nanotube is added to VNitric acid: VSulfuric acidIt is ultrasonic in the nitration mixture of=3:1, in stirring speed Degree is 300~500 revs/min, 3~5h of reflux under the conditions of temperature is 40~90 DEG C, and washing is to neutrality after natural cooling, at 60 DEG C It is dried in vacuo 6~12 hours under the conditions of~80 DEG C, obtains pretreated carbon nanotube acidification grafting oxygen-containing group;
(2) pretreated carbon nanotube is added in ethanol solution, 0.5~1h homogenous disperse is ultrasonically treated, by nitric acid Silver dissolves in ultrapure water as silver-colored presoma obtains silver nitrate solution, and dissolution in ultrapure water is added in sodium hydroxide and obtains hydrogen-oxygen Change sodium solution, after the ethanol solution of silver nitrate solution and carbon nanotube is uniformly mixed, sodium hydroxide solution, mixing is added dropwise Uniformly, it is transferred in ptfe autoclave, 20~30h of reaction at 140 DEG C~190 DEG C, after natural cooling, washs into Property is dried in vacuo 6~12 hours under the conditions of 60 DEG C~80 DEG C and obtains high thermal conductivity lubricating additive.
Prepared composite material is added in lubricating oil or lubricating grease according to Different adding amount, if being added to lubricating grease In can use three-roll grinder homogenous disperse.
Compared with prior art, the invention has the following beneficial effects: the additives of the carbon nanotube loaded silver of preparation can The dispersion performance for improving carbon nanotube, is preferably dispersed in lubricating grease and lubricating oil, can be used as grease additive use.System Standby carbon nanotube loaded silver additive is high heat-conductivity conducting composite material, has excellent mechanical property and antiwear and antifriction Energy.It is added in lubricating oil and lubricating grease, the thermal coefficient and lubricating oil and lubricating grease of lubricating oil and lubricating grease can be greatly promoted Frictional behaviour.The preparation method of high thermal conductivity lubricating additive is simple to operation, and comprehensive performance is strong, and addition uses simple and convenient, With good service performance.
Detailed description of the invention
Fig. 1 is the TEM figure of institute's product in embodiment 1.
Specific embodiment
Technical effect of the invention is further illustrated with attached drawing with reference to embodiments.
Embodiment 1:
Carbon nanotube and nano Silver quality ratio are 10:1, and carbon nanotube is added to V firstNitric acid: VSulfuric acidIn the nitration mixture of=3:1 Ultrasonic 0.5h, low whipping speed are 500 revs/min, and temperature flows back 5h under the conditions of being 50 DEG C, after natural cooling washing to neutrality, It is dried in vacuo 12 hours under the conditions of 60 DEG C, obtains pretreated carbon nanotube.The pretreated carbon nanotube of 1g is added to In ethanol solution, it is ultrasonically treated 0.5h homogenous disperse, takes 0.157g silver nitrate to dissolve in the ultrapure water of 10mL and obtains silver nitrate Solution takes the sodium hydroxide of 0.3g that dissolution in the ultrapure water of 10mL is added and obtains sodium hydroxide solution, by silver nitrate solution and carbon After the ethanol solution of nanotube is uniformly mixed, sodium hydroxide solution is added dropwise, is uniformly mixed, is transferred to polytetrafluoroethyl-ne alkene reaction In kettle, 20h is reacted at 160 DEG C, after natural cooling, with milli-Q water to neutrality, be dried in vacuo 12 hours under the conditions of 60 DEG C To composite material.Composite material is passed through into milled processed, is shown according to measurement result and dimethyl is added to 30wt% additive amount In silicone oil, thermal conductivity ratio dimethicone increases to 6 times of original coefficient, is added in silicone grease with 10wt% additive amount, Its fretting wear coefficient is reduced to the 1/2 of original coefficient, and wear scar diameter decreases 1.73 times.
Table 1 is the delta data that embodiment 1 is added to obtained thermal coefficient in dimethicone;Table 2 is embodiment 1 The greasy property delta data being added in lubricating grease.
Table 1
Dimethicone 30wt%Ag/CNT dimethicone
Thermal coefficient λ/(W/m*K)-1 0.1516 0.9096
Table 2
Silicone grease 10wt%Ag/CNT silicone grease
Coefficient of friction 0.097 0.052
Wear scar diameter (mm) 0.972 0.563
Embodiment 2:
Carbon nanotube and nano Silver quality ratio are 5:1, and carbon nanotube is added to V firstNitric acid: VSulfuric acidIn the nitration mixture of=3:1 Ultrasonic 0.5h, low whipping speed are 400 revs/min, and temperature flows back 4h under the conditions of being 90 DEG C, after natural cooling washing to neutrality, It is dried in vacuo 6 hours under the conditions of 80 DEG C, obtains pretreated carbon nanotube.The pretreated carbon nanotube of 1g is added to second In alcoholic solution, it is ultrasonically treated 1h homogenous disperse, takes 0.315g silver nitrate to dissolve in the ultrapure water of 10mL and obtains silver nitrate solution, Dissolution in ultrapure water is added in 0.4g sodium hydroxide and obtains sodium hydroxide solution, the ethyl alcohol of silver nitrate solution and carbon nanotube is molten After liquid is uniformly mixed, sodium hydroxide solution is added dropwise, is uniformly mixed, is transferred in ptfe autoclave, it is anti-at 180 DEG C Answer 26h, after natural cooling, washing to neutrality is dried in vacuo 10 hours under the conditions of 80 DEG C and obtains composite material.Composite material is passed through Milled processed is crossed, shows that thermal coefficient increases to original with 20wt% additive amount into No. 2 lithium base basis rouge according to measurement result 7 times for carrying out coefficient, are added in dimethicone with 10wt% additive amount, and fretting wear coefficient and wear scar diameter all substantially drop As low as the 1/2 of original coefficient.
Table 3 is the delta data that embodiment 2 is added to obtained thermal coefficient in dimethicone;Table 4 is embodiment 2 The greasy property delta data being added in lubricating grease.
Table 3
Dimethicone 30wt%Ag/CNT dimethicone
Thermal coefficient λ/(W/m*K)-1 0.1516 1.0612
Table 4
Silicone grease 10wt%Ag/CNT silicone grease
Coefficient of friction 0.097 0.049
Wear scar diameter (mm) 0.972 0.489
Embodiment 3:
Carbon nanotube and nano Silver quality ratio are 10:3, and carbon nanotube is added to V firstNitric acid: VSulfuric acidIn the nitration mixture of=3:1 Ultrasonic 0.5h, low whipping speed are 400 revs/min, and temperature flows back 4h under the conditions of being 90 DEG C, after natural cooling washing to neutrality, It is dried in vacuo 6 hours under the conditions of 80 DEG C, obtains pretreated carbon nanotube.The pretreated carbon nanotube of 1g is added to second In alcoholic solution, it is ultrasonically treated 1h homogenous disperse, takes 0.472g silver nitrate to dissolve in the ultrapure water of 10mL and obtains silver nitrate solution, Dissolution in ultrapure water is added in 0.4g sodium hydroxide and obtains sodium hydroxide solution, the ethyl alcohol of silver nitrate solution and carbon nanotube is molten After liquid is uniformly mixed, sodium hydroxide solution is added dropwise, is uniformly mixed, is transferred in ptfe autoclave, it is anti-at 180 DEG C Answer 26h, after natural cooling, washing to neutrality is dried in vacuo 10 hours under the conditions of 80 DEG C and obtains composite material.Composite material is passed through Milled processed is crossed, shows that thermal coefficient increases to original with 20wt% additive amount into No. 2 lithium base basis rouge according to measurement result 5 times for carrying out coefficient, are added in dimethicone with 10wt% additive amount, and fretting wear coefficient is reduced to the 2/ of original coefficient 3, wear scar diameter is also reduced to the 1/2 of original coefficient.
Table 5 is the delta data that embodiment 3 is added to obtained thermal coefficient in dimethicone;Table 6 is embodiment 3 The greasy property delta data being added in lubricating grease.
Table 5
Dimethicone 30wt%Ag/CNT dimethicone
Thermal coefficient λ/(W/m*K)-1 0.1516 0.763
Table 6
Silicone grease 10wt%Ag/CNT silicone grease
Coefficient of friction 0.097 0.065
Wear scar diameter (mm) 0.972 0.562
Comparative example 1:
The preparation of pure nano silver takes 3.14g silver nitrate to dissolve in the ultrapure water of 10mL and obtains silver nitrate solution, by 0.4g Sodium hydroxide is added dissolution in ultrapure water and obtains sodium hydroxide solution, and sodium hydroxide solution is added dropwise in silver nitrate solution, mixes Uniformly, it is transferred in ptfe autoclave, reacts 26h at 180 DEG C, after natural cooling, washing to neutrality, under the conditions of 80 DEG C Vacuum drying obtains composite material in 10 hours.Nano silver is passed through into milled processed, is shown according to measurement result and is added with 20wt% It measures into No. 2 lithium base basis rouge, thermal coefficient increases to 2 times of original coefficient, is added to dimethyl with 10wt% additive amount In silicone oil, fretting wear coefficient is reduced to the 3/4 of original coefficient, and wear scar diameter is also reduced to original 4/5.
Table 7 is the delta data that comparative example 1 is added to obtained thermal coefficient in dimethicone;Table 8 is comparative example 1 The greasy property delta data being added in lubricating grease.
Table 7
Dimethicone 30wt%Ag/CNT dimethicone
Thermal coefficient λ/(W/m*K)-1 0.1516 0.3031
Table 8
Silicone grease 10wt%Ag/CNT silicone grease
Coefficient of friction 0.097 0.072
Wear scar diameter (mm) 0.972 0.774
Table 9
Table 9 is the delta data that embodiment 1,2,3 and comparative example 1 are added to obtained thermal coefficient in dimethicone And its greasy property delta data in lubricating grease.
From data it can be seen that the heating conduction and anti-wear and wear-resistant performance of embodiment 2 are optimal.The reason is that Nano silver grain The advantage for the high aspect ratio that has with excellent heating conduction and carbon pipe itself, which combines, can greatly promote the thermally conductive of material Performance.When Nano silver grain is less its heating conduction increase it is unobvious, to it is a certain amount of when reach optimum proportioning 5:1, when more It is easy to reunite, pure nano silver is then easy to reunite can not to form thermal conducting path.The mechanical property that carbon pipe itself has can promote lubrication The anti-wear and wear-resistant performance of rouge.

Claims (4)

1. a kind of high thermal conductivity lubricating additive, which is characterized in that be made of carbon nanotube and nano silver.
2. high thermal conductivity lubricating additive as described in claim 1, which is characterized in that the quality of the carbon nanotube and nano silver Proportion is respectively 5-10:1-3.
3. high thermal conductivity lubricating additive as described in claim 1, which is characterized in that the quality of the carbon nanotube and nano silver Proportion is respectively 10:1,5:1,10:3.
4. the preparation method of high thermal conductivity lubricating additive described in claim 1, it is characterised in that include the following steps:
(1) carbon nanotube acidification is handled: carbon nanotube is added to VNitric acid: VSulfuric acidUltrasonic in the nitration mixture of=3:1, low whipping speed is 300 ~ 500 revs/min, temperature flows back 3 ~ 5h under the conditions of being 40 ~ 90 DEG C, and washing is to neutrality after natural cooling, in 60 DEG C ~ 80 DEG C items It is dried in vacuo 6 ~ 12 hours under part, obtains pretreated carbon nanotube acidification grafting oxygen-containing group;
(2) pretreated carbon nanotube is added in ethanol solution, be ultrasonically treated 0.5 ~ 1h homogenous disperse, using silver nitrate as Silver-colored presoma dissolves in ultrapure water obtains silver nitrate solution, and it is molten that dissolution in sodium hydroxide addition ultrapure water is obtained sodium hydroxide Liquid after being uniformly mixed the ethanol solution of silver nitrate solution and carbon nanotube, is added dropwise sodium hydroxide solution, is uniformly mixed, It is transferred in ptfe autoclave, 20 ~ 30h of reaction at 140 DEG C ~ 190 DEG C, after natural cooling, washing to neutrality, 60 DEG C ~ It is dried in vacuo 6 ~ 12 hours under the conditions of 80 DEG C and obtains high thermal conductivity lubricating additive.
CN201910149943.3A 2019-02-28 2019-02-28 A kind of high thermal conductivity lubricating additive and preparation method thereof Pending CN109825344A (en)

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CN116536094A (en) * 2022-12-29 2023-08-04 天津职业技术师范大学(中国职业培训指导教师进修中心) Lubricating oil containing nano silver/metal organic framework additive and preparation method thereof

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110964588A (en) * 2019-10-30 2020-04-07 惠州学院 High-conductivity lubricating additive and preparation method and application thereof
CN116536094A (en) * 2022-12-29 2023-08-04 天津职业技术师范大学(中国职业培训指导教师进修中心) Lubricating oil containing nano silver/metal organic framework additive and preparation method thereof

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Application publication date: 20190531