CN107338086A - Lube oil additive of graphene doped and compounded dispersant and preparation method thereof - Google Patents

Lube oil additive of graphene doped and compounded dispersant and preparation method thereof Download PDF

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Publication number
CN107338086A
CN107338086A CN201710657192.7A CN201710657192A CN107338086A CN 107338086 A CN107338086 A CN 107338086A CN 201710657192 A CN201710657192 A CN 201710657192A CN 107338086 A CN107338086 A CN 107338086A
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graphene
lubricating oil
dispersant
compounded
preparation
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CN201710657192.7A
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Inventor
常珈瑞
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Chongqing Huayang Graphene Technology Co Ltd
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Chongqing Huayang Graphene Technology Co Ltd
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Priority to CN201710657192.7A priority Critical patent/CN107338086A/en
Publication of CN107338086A publication Critical patent/CN107338086A/en
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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
    • C10M161/00Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
    • 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
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
    • 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
    • C10M2201/14Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
    • 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
    • C10M2215/00Organic non-macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2215/28Amides; Imides
    • 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
    • C10M2217/00Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/06Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
    • 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
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure

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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 discloses a kind of lube oil additive of graphene doped and compounded dispersant and preparation method thereof, belong to new material and its application field, be mainly used in performance improvement and the raising of lubricating oil.It is characterized in that:Single or multiple lift graphene and specific composite dispersing agent are added in lubricating oil by the method for in-situ modification, ultrasonic disperse, by reducing sedimentation and the agglomeration traits of graphene, play anti-wear and wear-resistant performance of the graphene in lubricating oil.Mass percentage content of the described single or multiple lift graphene in lubricating oil is 0.001 0.8%;Mass percentage content of the described composite dispersing agent in lubricating oil is 0.01 2%.By preferably finding in the present invention, after the graphene of two kinds of particle size ranges and two kinds of dispersants doping, the synthesis tribological property of formation testing can be improved, antifriction and wear resistence reach optimum state simultaneously.

Description

Lube oil additive of graphene doped and compounded dispersant and preparation method thereof
Technical field
The invention discloses a kind of novel lubricating oil additive based on graphene doping high efficiency composition dispersant, belong to new Material and its application field, it is mainly used in performance improvement and the raising of lubricating oil.
Background technology
Fretting wear is prevalent in industry-by-industry, due to loss caused by friction account for the 50% of world's primary energy with On, while the abrasion between rubbing surface is also one of the main reason for material and facility is scrapped in industry-by-industry.Therefore in machinery Add lubricating oil be generally using a kind of reduction fretting wear by the way of.In order to improve the anti-wear and wear-resistant performance of lubricating oil, lead to It is often that various antifriction and antiwear agentses are added in lubricating oil.
Graphene is a kind of two-dimensional structure with atomic layer level thickness, has excellent mechanical property, single or multiple lift Graphene has ultra-thin lamellar structure.Present graphene research is it has been found that its excellent self lubricity adds in lubrication Agent field will have broad application prospects.But because graphene is solid particle, the dispersion stabilization in oil is not good enough, therefore is moistening Sedimentation and agglomeration are easily produced in lubricating oil, so as to limit its application as antiwear and friction-reducing additive.
The content of the invention
In view of this, an object of the present invention is to provide a kind of novel lubricating based on graphene doped and compounded dispersant Oil additive, it is therefore an objective to solve agglomeration of the graphene in lubricating oil, dispersion stabilization be improved, so as to give full play to it Anti-wear and wear-resistant performance.To achieve the above object, the present invention specifically provides following technical scheme:By single or multiple lift graphene Added with composite dispersing agent by the method for in-situ modification, ultrasonic disperse in lubricating oil, by the sedimentation and the group that reduce graphene Poly- problem, play anti-wear and wear-resistant performance of the graphene in lubricating oil.
Mass percentage content of the described single or multiple lift graphene in lubricating oil is 0.001-0.8%;Described height It is 0.01-2% to imitate mass percentage content of the composite dispersing agent in lubricating oil.
The particle size range of described single or multiple lift graphene is 5-150 μm, needs to add in lubricating oil in above-mentioned grain The graphene of one or more of different-grain diameters in the range of footpath;Described single or multiple lift graphene is by " method from top to bottom " Or " method from bottom to top " is prepared;The ratio surface of described single or multiple lift graphene is 150-2630 m2/ g, single graphite The thickness of alkene piece is 0.34-10 nm.
Described composite dispersing agent is detergent-dispersant additive, including mono alkenyl succimide(T151), the double fourths of polyisobutene Imidodicarbonic diamide(T154), polyisobutylene succinamide(T155)With high molecular weight polyisobutylene succimide(T161)In One or more.
Described lubricating oil be mineral base oil, synthetic base oil, any commercialization or homemade lubricating oil one kind or It is several.
Described single or multiple lift graphene is with composite dispersing agent using in-situ modification, the method for ultrasonic disperse to graphene Surface is doped modification, and polyisobutylene group is introduced on the benzene hexatomic ring of graphene and forms steric hindrance, hinders graphene The reunion of particle, include following preparation process:(1) use in-situ modification method by high efficiency composition dispersant-coated in graphene table Graphene after modification and high efficiency composition dispersant are dispersed in lubricating oil by face, (2) by ultrasonic dispersion.
Further, the in-situ modification method of the step (1), includes following preparation process:1) by 1 part of mass fraction Single or multiple lift graphene is dissolved in volume ratio for 1:1-1:In 3 water and the solvent of absolute ethyl alcohol, the mixed of 3-15 mg/mL is made into Solution is closed, is added in oblique type three neck round bottom flask, and heated in 50-80 DEG C of water-bath;2) by the compound of 3-7 part mass fractions Dispersant is added in separatory funnel, and the mixed solution of graphene-containing is added with d/ points of speed of 15-40, and with 300-700 Rev/min speed stirring reaction 40-80 minutes;3) after stirring terminates, reaction solution is poured out from oblique type three neck round bottom flask, used Buchner funnel filters product vacuum, with absolute ethyl alcohol washed product 3 times;4) product after washing is moved in surface plate, is utilized For vacuum drying chamber in 30-50 DEG C of temperature, vacuum dries 20-36 h under conditions of being the MPa of -0.07 MPa ~ -0.09.
Further, the ultra-sonic dispersion method of the step (2) is:Graphite after step (1) is modified by in-situ method Alkene and high efficiency composition dispersant are added in lubricating oil, are 800-1200 W in power, under the conditions of tranmitting frequency is 20-35 kHz, Water bath sonicator vibrates 8-15 minutes.
Further, the single or multiple lift graphene that added in lubricating oil is two kinds of different-grain diameter of addition simultaneously The graphite that the graphene and particle size range that single or multiple lift graphene, respectively particle size range are 10-30 μm are 70-130 μm Mass percentage content of the graphene that alkene, wherein particle diameter are 10-30 μm in lubricating oil is 0.005-0.4%, particle diameter 70- The mass percentage content in lubricating oil of 130 μm of graphene is 0.005-0.4%;Described being added in lubricating oil is efficient Composite dispersing agent is adds two kinds of high efficiency composition dispersants, respectively T154 and T161 simultaneously, and wherein T154 is in lubricating oil Mass percentage content is 0.05-1.0%, and mass percentage contents of the T161 in lubricating oil is 0.05-1.0%.
Preferably, mass percentage content of the graphene that described particle diameter is 10-30 μm in lubricating oil is 0.01%, The mass percentage content in lubricating oil for the graphene that particle diameter is 80-120 μm is quality of 0.1%, the T154 in lubricating oil Degree is that mass percentage contents of 0.1%, the T161 in lubricating oil is 0.1%.The optimization formula provided forms: 0.01%(10-30 μm of graphene)+0.1%(70-130 μm of graphene)+ 0.1%-T154+0.1%-T161+99.69% blank oil.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below:
Fig. 1 is the coefficient of friction and wear scar diameter of the lube oil additive of the different component of embodiment 1.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.It is unreceipted specific in embodiment The experimental method of condition, generally according to normal condition or according to the condition proposed by manufacturer.
Embodiment 1
Based on the novel lubricating oil additive of graphene doping high efficiency composition dispersant, prepare 5 kinds of formation testings as shown in table 1 and rubbed Wipe wear testing.
Table 1:The formation testing of different component.
Graphene, dispersant and lubricating oil, ultrasound 10 minutes, using MRS-1J are weighed according to said components mass percent The method that type abrasion tester is tested by four balls determines coefficient of friction and wear scar diameter, resists so as to evaluate formation testing 1-5 antifriction Grind performance.The friction pair way of contact is ball-ball point contact, and the steel ball used is four-ball tester special-purpose steel ball (material GCr15, size 12.7mm, 59-61HRC of Rockwell Hardness), the experiment condition used is load 392N, rotating speed 1200r/min, time 60min.
It can be seen from Fig. 1, compared with blank formation testing 1, the antifriction of formation testing 5 improves 46.7%, wear-resistant to improve 9.8%, two The graphene of kind of particle size range antifriction and resists with that after two kinds of dispersant with high efficiency doping, can improve the synthesis tribological property of formation testing Mill property reaches optimum state simultaneously.The graphene of two kinds of different-grain diameters is compounded or individually can not with two kinds of dispersant with high efficiency doping The anti-wear and wear-resistant performance of formation testing is set to reach optimum state, the additive formulations of formation testing 5 are optimization formula, and formula composition is:0.01% (10-30 μm of graphene)+0.1%(70-130 μm of graphene)+ 0.1%-T154+0.1%-T161+99.69% blank oil.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be Various changes are made to it in form and in details, without departing from claims of the present invention limited range.

Claims (9)

1. lube oil additive of graphene doped and compounded dispersant and preparation method thereof, it is characterised in that:Add in lubricating oil Enter single or multiple lift graphene and high efficiency composition dispersant;Quality percentage of the described single or multiple lift graphene in lubricating oil It is 0.001-0.8% than content;Mass percentage content of the described high efficiency composition dispersant in lubricating oil is 0.01-2%.
2. lube oil additive of graphene doped and compounded dispersant according to claim 1 and preparation method thereof, it is special Sign is:The particle size range of described single or multiple lift graphene is 5-150 μm, needs to add in lubricating oil in above-mentioned grain The graphene of one or more of different-grain diameters in the range of footpath;Described single or multiple lift graphene is by " method from top to bottom " Or " method from bottom to top " is prepared;The ratio surface of described single or multiple lift graphene is 150-2630 m2/ g, single graphite The thickness of alkene piece is 0.34-10 nm.
3. lube oil additive of graphene doped and compounded dispersant according to claim 1 and preparation method thereof, it is special Sign is:Described composite dispersing agent is detergent-dispersant additive, including mono alkenyl succimide(T151), the double fourths two of polyisobutene Acid imide(T154), polyisobutylene succinamide(T155)With high molecular weight polyisobutylene succimide(T161)In It is one or more of.
4. lube oil additive of graphene doped and compounded dispersant according to claim 1 and preparation method thereof, it is special Sign is:Described lubricating oil is one kind or several of mineral base oil, synthetic base oil, any commercialization or homemade lubricating oil Kind.
5. lube oil additive and its preparation side of the graphene doped and compounded dispersant according to claim any one of 1-4 Method, it is characterised in that:Single or multiple lift graphene is with composite dispersing agent using in-situ modification, the method for ultrasonic disperse to graphene Surface is doped modification, and polyisobutylene group is introduced on the benzene hexatomic ring of graphene and forms steric hindrance, hinders graphene The reunion of particle, include following preparation process:(1) use in-situ modification method by high efficiency composition dispersant-coated in graphene table Graphene after modification and composite dispersing agent are dispersed in lubricating oil by face, (2) by ultrasonic dispersion.
6. lube oil additive of graphene doped and compounded dispersant according to claim 5 and preparation method thereof, it is special Sign is:The in-situ modification method of the step (1), includes following preparation process:1) by the single or multiple lift of 1 part of mass fraction Graphene is dissolved in volume ratio for 1:1-1:In 3 water and the solvent of absolute ethyl alcohol, 3-15 mg/mL mixed solution is made into, is added Into oblique type three neck round bottom flask, and heated in 50-80 DEG C of water-bath;2) composite dispersing agent of 3-7 part mass fractions is added Into separatory funnel, the mixed solution of graphene-containing is added with d/ points of speed of 15-40, and with 300-700 revs/min of speed Stirring reaction 40-80 minutes;3) after stirring terminates, reaction solution is poured out from oblique type three neck round bottom flask, will with Buchner funnel Product vacuum filters, with absolute ethyl alcohol washed product 3 times;4) product after washing is moved in surface plate, utilizes vacuum drying chamber In 30-50 DEG C of temperature, vacuum dries 20-36 h under conditions of being the MPa of -0.07 MPa ~ -0.09.
7. lube oil additive of graphene doped and compounded dispersant according to claim 5 and preparation method thereof, it is special Sign is:The ultra-sonic dispersion method of the step (2) is:Graphene after step (1) is modified by in-situ method and efficiently multiple Close dispersant to add in lubricating oil, be 800-1200 W in power, under the conditions of tranmitting frequency is 20-35 kHz, water bath sonicator shakes Swing 8-15 minutes.
8. lube oil additive and its preparation side of the graphene doped and compounded dispersant according to claim any one of 1-7 Method, it is characterised in that:Described adds single or multiple lift graphene to add the list of two kinds of different-grain diameters simultaneously in lubricating oil Layer or multi-layer graphene, the graphene that the graphene and particle size range that respectively particle size range is 10-30 μm are 70-130 μm, Mass percentage content of the graphene that wherein particle diameter is 10-30 μm in lubricating oil is 0.005-0.4%, particle diameter 70-130 μm the mass percentage content in lubricating oil of graphene be 0.005-0.4%;Described adds composite diffusion in lubricating oil To add two kinds of composite dispersing agents simultaneously, the mass percent of respectively T154 and T161, wherein T154 in lubricating oil contains for agent It is 0.05-1.0% to measure as 0.05-1.0%, mass percentage contents of the T161 in lubricating oil.
9. lube oil additive of graphene doped and compounded dispersant according to claim 8 and preparation method thereof, it is special Sign is:Mass percentage content of the graphene that described particle diameter is 10-30 μm in lubricating oil is 0.01%, and particle diameter is The mass percentage content in lubricating oil of 70-130 μm of graphene is mass percents of 0.1%, the T154 in lubricating oil Content is that mass percentage contents of 0.1%, the T161 in lubricating oil is 0.1%.
CN201710657192.7A 2017-08-03 2017-08-03 Lube oil additive of graphene doped and compounded dispersant and preparation method thereof Pending CN107338086A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109135898A (en) * 2018-10-31 2019-01-04 黑龙江莱弗力通科技有限公司 A kind of graphene lubricating oil composite dispersing agent and preparation method thereof
CN109536261A (en) * 2018-12-24 2019-03-29 山东陆邦石化有限公司 Peace and quiet type lubricating oil of extreme-pressure anti-wear and preparation method thereof
CN110699152A (en) * 2019-11-20 2020-01-17 法尔胜泓昇集团有限公司 Modified grease for enhancing wear resistance and extrusion resistance of steel wire rope and preparation method thereof
CN112852523A (en) * 2021-03-09 2021-05-28 上海通原环保科技有限公司 Renewable lubricating oil composition based on graphene modification

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812351A (en) * 2010-04-01 2010-08-25 江苏工业学院 Lubricating oil additive based on single-layer or more-layer graphene
CN102911762A (en) * 2012-11-02 2013-02-06 上海第二工业大学 High-thermal conductivity lubricating oil and preparation method thereof
CN106190432A (en) * 2016-07-07 2016-12-07 重庆德领科技有限公司 A kind of modified graphene lubricating oil of polymolecularity and preparation method thereof
CN106244289A (en) * 2016-07-07 2016-12-21 重庆德领科技有限公司 Dispersibility and the good modified graphene lubricating oil of affinity and preparation method thereof
CN106811267A (en) * 2015-12-02 2017-06-09 中国科学院宁波材料技术与工程研究所 Graphene modified HMW ashless dispersant, its preparation method and application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101812351A (en) * 2010-04-01 2010-08-25 江苏工业学院 Lubricating oil additive based on single-layer or more-layer graphene
CN102911762A (en) * 2012-11-02 2013-02-06 上海第二工业大学 High-thermal conductivity lubricating oil and preparation method thereof
CN106811267A (en) * 2015-12-02 2017-06-09 中国科学院宁波材料技术与工程研究所 Graphene modified HMW ashless dispersant, its preparation method and application
CN106190432A (en) * 2016-07-07 2016-12-07 重庆德领科技有限公司 A kind of modified graphene lubricating oil of polymolecularity and preparation method thereof
CN106244289A (en) * 2016-07-07 2016-12-21 重庆德领科技有限公司 Dispersibility and the good modified graphene lubricating oil of affinity and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109135898A (en) * 2018-10-31 2019-01-04 黑龙江莱弗力通科技有限公司 A kind of graphene lubricating oil composite dispersing agent and preparation method thereof
CN109536261A (en) * 2018-12-24 2019-03-29 山东陆邦石化有限公司 Peace and quiet type lubricating oil of extreme-pressure anti-wear and preparation method thereof
CN110699152A (en) * 2019-11-20 2020-01-17 法尔胜泓昇集团有限公司 Modified grease for enhancing wear resistance and extrusion resistance of steel wire rope and preparation method thereof
CN112852523A (en) * 2021-03-09 2021-05-28 上海通原环保科技有限公司 Renewable lubricating oil composition based on graphene modification
CN112852523B (en) * 2021-03-09 2022-12-06 山东莱克科技有限公司 Renewable lubricating oil composition based on graphene modification

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