CN103113958A - Preparation method of graphene alkenyl nano-copper lubricant additive - Google Patents
Preparation method of graphene alkenyl nano-copper lubricant additive Download PDFInfo
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- CN103113958A CN103113958A CN2013100685165A CN201310068516A CN103113958A CN 103113958 A CN103113958 A CN 103113958A CN 2013100685165 A CN2013100685165 A CN 2013100685165A CN 201310068516 A CN201310068516 A CN 201310068516A CN 103113958 A CN103113958 A CN 103113958A
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Abstract
The invention discloses a preparation method of a graphene alkenyl nano-copper lubricant additive. The method comprises the following steps: dispersing oxidized graphene serving as a raw material into deionized water to carry out an ultrasonic treatment; adding a copper salt solution mixed with a surfactant and carrying out an ultrasonic intercalating treatment; carrying out a water-bath treatment on the mixed oxidized graphene copper salt solution and a concentrated ammonium solution of hydrazine hydrate, then adding a proper amount of ascorbic acid; pouring the mixed solution into a stainless steel reactor kettle with a polytetrafluoroethylene liner; reacting for a period of time at a set temperature and then naturally cooling; cleaning the reaction product in a suction filtering manner for many times by using the deionized water and ethanol; and drying the product, thus obtaining the graphene alkenyl nano-copper additive. The graphene alkenyl nano-copper additive can be added into various industrial lubricants so that the lubricants have excellent using performances. Therefore, the friction is decreased obviously. As a result, the service life of a machine, equipment or a component part is prolonged effectively.
Description
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Technical field
The present invention relates to nano inorganic functional materials preparing technical field, relate in particular to a kind of graphene-based nano copper lubricating oil additive material preparation method.
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Background technology
Energy and environment are two principal themes of economic society sustainable development.For component of machine, frictional wear is can hardly be avoided.The frictional wear of mechanical part also can cause very serious environmental pollution when bringing a large amount of losses of material and the energy.Adding triboadditives in lubricating oil is one of important technical of effectively slowing down component of machine frictional wear, reduction energy waste.
In recent years, the preparation and application technology of nano metal material has obtained significant progress, has reached gradually the level that industrialization generates.The nano-metal particle material refers to that geometrical dimension is the metal ultrafine particle of 1-100nm level, be between single atom and solid-state between the atom set body.Nearest result of study discovery, the nano-metal particle material has a good application prospect as lubricating oil additive, so be born many technology and products based on this kind novel material.But the research that at present the nano metal matrix material is applied to lubricating oil additive has no report, and for this reason, we have studied graphene-based Nanometer Copper matrix material is used for lubricating oil additive, and have studied the preparation method of this additive material.
Graphene is the new carbon with monatomic bed thickness, and it has high physical strength, and good thermal conductivity and carrier mobility fast are for the preparation of the contour performance device of transistor sensor provides raw material.In addition, Graphene has high specific surface area, is the fabulous base material of preparation nano composite material.
Metal nanoparticle has attracted to study widely interest due to electricity, optics and the catalytic performance of uniqueness.These character of research discovery nano particle and its appearance and size grain spacing etc. have substantial connection, Graphene can effectively limit the growth of metallic particles as a kind of nano material simple in structure, make it obtain the less nano-sized particles of homogeneous.Can be in the nano material substrate well disperse by the resize ratio metal nanoparticle, suppressed their reunion, make it have higher specific surface area, higher reactive behavior and selectivity.
Yet the method for preparing at present Graphene-copper nano composite material is comparatively complicated single.At present disclosed have the stability that improves graphene film by anion surfactant, and promote the method (Nano Letters is open in 2004) of metal oxide self-assembled growth on graphene film of copper.And by reduction CuCl
2The intercalated graphite mixture prepares Graphene encapsulation copper nano composite material (J. Phys.Chem. Solids is open in 2009).Utilize in addition the reducing flame technology copper nano particles is deposited on ~ the thick graphene platelet of 3nm on (Nanotechnology is open in 2008).Because Graphene shell in these methods is to protect copper nanometer core not oxidized, so the copper nano composite material of this Graphene encapsulation is difficult to make its application performance to reach maximization.Although about the certain open basis of having of Graphene copper nano-particle matrix material, used poisonous strong reductant sodium borohydride but above-mentioned disclosed Graphene copper nano-particle composite material and preparation method thereof has, have plenty of and carry out under the severe corrosive condition, and also openly do not adopt hydrothermal method to prepare the research of graphene-based copper nano composite material at present.
The present invention has introduced a kind of graphene-based nano copper lubricating oil additive material preparation method, have the following advantages (1) go to improve the system reducing ability with the reduction group that mixes, keep simultaneously gentle reaction environment (2) to guarantee that by the consumption of controlling reductive agent graphene oxide and copper nano particles change the accumulation that the deposition of (3) copper nano particles on graphene film can greatly reduce graphene nanometer sheet simultaneously.(4) can realize the controlled of copper nano-particle pattern adding of tensio-active agent.This additive material adds in lubricating oil, can show excellent anti-wear and wear-resistant performance, thereby effectively delays the work-ing life of friction pair.
Summary of the invention
The purpose of this invention is to provide a kind of graphene-based nano copper lubricating oil additive material preparation method.The method is take graphite oxide and mantoquita as raw material, adopt xitix and a small amount of hydrazine hydrate as the associating reductive agent, while reduced graphene oxide serving and cupric ion, obtain graphene-based nanometer copper particle material under hydrothermal reaction condition, and this preparation method is simple, convenient, efficient.
Technical scheme of the present invention is as follows:
(a) graphene oxide is synthetic: be raw material with natural graphite, add a certain amount of vitriol oil, SODIUMNITRATE to stir for some time in ice bath, then slowly add a certain amount of potassium permanganate, after potassium permanganate dissolves fully, reaction system is transferred to 35 ℃ of stirred in water bath react half an hour, join slowly a certain amount of deionized water in reaction system, continue to stir, add again a certain amount of superoxol, at last with mentioned solution centrifuging, repeatedly be washed with water to neutrality, drying can make graphene oxide;
(b) aqueous solution of (1) preparation graphene oxide: the ratio of graphene oxide with 1mg/mL-2mg/mL is distributed in deionized water supersound process 30-90min;
(2) a certain amount of copper sulfate and tensio-active agent are dissolved in ultrasonic 10-30min in distilled water, then mix with solution (1), and ultrasonic 30-60min;
(3) liquor ammoniae fortis with appropriate hydrazine hydrate slowly adds in the mixing solutions of step (2) preparation, at a certain temperature the stirring in water bath appropriate time;
(4) appropriate xitix is joined in the prepared solution of step (3), pour into in the teflon-lined stainless steel cauldron, naturally cooling after 80-120 ℃ of reaction 2-5h;
(5) utilize deionized water, ethanol repeatedly to wash suction filtration to reaction product after, drying obtains graphene-based Nano-Cu Additive material.
Wherein mantoquita is that the concentration of copper sulfate is 2-5mg/mL in step (2), and tensio-active agent is disodium ethylene diamine tetraacetate;
Wherein in the liquor ammoniae fortis of the middle hydrazine hydrate of step (3), the volume ratio of hydrazine hydrate and ammoniacal liquor is 1:2; Bath temperature is 30-50 ℃, time 30-60min;
That the present invention has is simple and easy to do, rapidly and efficiently, the advantage such as technique is simple, adopt the reductive agent that mixes, copper nano-particle size homogeneous (20nm left and right) in the matrix material of preparation, and can load to well on graphene sheet layer, the pattern that can realize copper nano particles is controlled, and can effectively prevent the reunion of Graphene.The synthetic graphene-based copper nano composite material of present method has potential using value at aspects such as electrochemical sensor and solid lubrication.
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Description of drawings
Fig. 1 is the X ray diffracting spectrum of the graphene-based Nano-Cu Additive material of embodiment 1 preparation;
Fig. 2 is the electron scanning micrograph of the graphene-based Nano-Cu Additive material of embodiment 1 preparation;
Fig. 3 is the electron scanning micrograph of the graphene-based Nano-Cu Additive material of embodiment 2 preparations;
Fig. 4 is that the prepared product of embodiment 1 adds the tribological property in base oil HVI500 to.
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Embodiment
Embodiment 1
The 50mg graphene oxide is distributed in the 50mL deionized water supersound process 30min; Be that 2mg/mL copper sulfate and 0.08g disodium ethylene diamine tetraacetate are dissolved in ultrasonic 10min in distilled water simultaneously with concentration, then mix with graphene oxide solution, and ultrasonic 60min; The liquor ammoniae fortis that with concentration is the hydrazine hydrate of 0.1mol/mL slowly adds in above-mentioned mixing solutions, at 30 ℃ of lower stirring in water bath 30min; Again appropriate xitix is added in solution, and pour into in the teflon-lined stainless steel cauldron, naturally cooling after 80 ℃ of reaction 5h; After utilizing deionized water, ethanol repeatedly to wash suction filtration to reaction product, drying obtains graphene-based Nanometer Copper nano composite material, is as shown in Figures 1 and 2 the X ray diffracting spectrum of the graphene-based Nano-Cu Additive material for preparing in the present embodiment and the photo of scanning electronic microscope.
Embodiment 2
The 100mg graphene oxide is distributed in the 50mL deionized water supersound process 30min; Be that 2mg/mL copper sulfate and 0.1g disodium ethylene diamine tetraacetate are dissolved in ultrasonic 10min in distilled water simultaneously with concentration, then mix with graphene oxide solution, and ultrasonic 30min; The liquor ammoniae fortis that with concentration is the hydrazine hydrate of 0.1mol/mL slowly adds in above-mentioned mixing solutions, at 30 ℃ of lower stirring in water bath 60min; Again appropriate xitix is added in solution, and pour into in the teflon-lined stainless steel cauldron, naturally cooling after 100 ℃ of reaction 2h; After utilizing deionized water, ethanol repeatedly to wash suction filtration to reaction product, drying obtains graphene-based Nanometer Copper nano composite material, and Fig. 3 is the electron scanning micrograph of the graphene-based Nano-Cu Additive material for preparing in the present embodiment.
Embodiment 3
The 100mg graphene oxide is distributed in the 100mL deionized water supersound process 30min; Be that 5mg/mL copper sulfate is dissolved in ultrasonic 10min in distilled water simultaneously with concentration, then mix with graphene oxide solution, and ultrasonic 60min; The liquor ammoniae fortis that with concentration is the hydrazine hydrate of 0.1mol/mL slowly adds in above-mentioned mixing solutions, at 50 ℃ of lower stirring in water bath 30min; Again appropriate xitix is added in solution, and pour into in the teflon-lined stainless steel cauldron, naturally cooling after 120 ℃ of reaction 2h; After utilizing deionized water, ethanol repeatedly to wash suction filtration to reaction product, drying obtains graphene-based Nanometer Copper nano composite material.
Embodiment 4
The graphene-based Nanometer Copper that embodiment 1 is prepared adds in base oil HVI750, wherein the content of graphene-based Nano-Cu Additive is 1%, ultra-sonic dispersion evenly after, use CETR UMT-2 frictional testing machines, investigate the MoSe2 that added with ball-dish pattern on the impact of base oil frictional behaviour.In experiment, disc used is the 45# steel, and diameter is 2 cm; Ball is the 440C stainless steel, and diameter is 10 mm; Rotating speed is 200 r/min, and the time is 30 min.
Fig. 4 is the prepared product of embodiment 1 during as additive, shows in figure that additive is to the influence curve of base oil HVI500 frictional behaviour.Wherein curve C 1 represents base oil HV1500, C2 represents and has added graphene-based Nano-Cu Additive in base oil HVI500, as can be seen from Figure, when with graphene-based Nanometer Copper during as additive, under the experiment condition of the present embodiment, the base oil HVI500 that has added graphene-based Nano-Cu Additive shows better frictional behaviour.
Need to prove; although technology contents of the present invention and technical characterictic have disclosed as above; yet those of ordinary skill in the art still may be based on teaching of the present invention and announcements and are done all replacement and modifications that does not deviate from spirit of the present invention; therefore; protection domain of the present invention should be not limited to the content that embodiment discloses; and should comprise various do not deviate from replacement of the present invention and modifications, and contained by the present patent application claim.
Claims (9)
1. the preparation method of a graphene-based nano copper lubricating oil additive, is characterized in that, comprises the steps:
(1) ratio of graphene oxide with 1mg/mL-2mg/mL is distributed in deionized water, and carries out the aqueous solution that supersound process obtains graphene oxide;
(2) a certain amount of copper sulfate and tensio-active agent are dissolved in ultrasonic in distilled water after, mix with solution in step (1), and carry out supersound process;
(3) liquor ammoniae fortis with appropriate hydrazine hydrate slowly adds in the mixing solutions of step (2) preparation, at a certain temperature the stirring in water bath appropriate time;
(4) appropriate xitix is joined in the prepared solution of step (3), pour in reactor, naturally cooling after reaction for some time under design temperature;
(5) utilize deionized water, ethanol repeatedly to wash suction filtration to reaction product after, drying obtains graphene-based nano copper lubricating oil additive.
2. the preparation method of graphene-based nano copper lubricating oil additive as claimed in claim 1, is characterized in that, the concentration of described copper sulfate is 2-5mg/mL.
3. the preparation method of graphene-based nano copper lubricating oil additive as claimed in claim 1, is characterized in that, described tensio-active agent is disodium ethylene diamine tetraacetate.
4. the preparation method of graphene-based nano copper lubricating oil additive as claimed in claim 1, is characterized in that, in the liquor ammoniae fortis of described hydrazine hydrate, the volume ratio of hydrazine hydrate and ammoniacal liquor is 1:2.
5. the preparation method of graphene-based nano copper lubricating oil additive as claimed in claim 1, is characterized in that, wherein in step (3), bath temperature is 30-50 ℃, and churning time is 30-60min.
6. the preparation method of graphene-based nano copper lubricating oil additive as claimed in claim 1, is characterized in that, in described step (1), the time of supersound process is 30-90min.
7. the preparation method of graphene-based nano copper lubricating oil additive as claimed in claim 1, is characterized in that, the reactor in described step (4) is with the teflon-lined stainless steel cauldron.
8. the preparation method of graphene-based nano copper lubricating oil additive as claimed in claim 1, it is characterized in that, in described step (2), a certain amount of copper sulfate and tensio-active agent are dissolved in ultrasonic 10-30min in distilled water, after solution in step (1) mixes, carry out supersound process 30-60min.
9. as the preparation method of the described graphene-based nano copper lubricating oil additive of claim 1 to 8 any one, it is characterized in that, in described step (4) in reactor under 80-120 ℃ the reaction 2-5h after naturally cooling.
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Cited By (8)
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| CN103769602A (en) * | 2014-01-23 | 2014-05-07 | 聊城大学 | Method for preparing nano-copper/graphene composite particles under assistance of ultrasonic wave |
| CN104479804A (en) * | 2014-11-25 | 2015-04-01 | 华南理工大学 | Nanometer copper/graphene composite material and preparation method and application thereof |
| CN105907444A (en) * | 2016-04-21 | 2016-08-31 | 济宁利特纳米技术有限责任公司 | Additive containing thiadiazole derivative, nano copper and graphene, preparation method of the additive, and lubricant oil containing the additive |
| RU2625453C1 (en) * | 2016-09-21 | 2017-07-14 | федеральное государственное бюджетное образовательное учреждение высшего образования "Донской государственный технический университет",(ДГТУ) | Additive for lubricants |
| CN108531240A (en) * | 2018-04-20 | 2018-09-14 | 厦门六烯科技有限公司 | A kind of graphene-based molybdenum sulfide nano antiwear agent and preparation method thereof |
| CN110624546A (en) * | 2019-10-22 | 2019-12-31 | 特烯（厦门）科技有限公司 | Preparation method of copper/graphene catalyst |
| CN113355146A (en) * | 2021-06-18 | 2021-09-07 | 西安工业大学 | Preparation method of graphene-loaded copper nanoparticles for lubricating oil additive |
| CN114131036A (en) * | 2021-12-03 | 2022-03-04 | 安徽工业大学 | Low-cost preparation method of functionalized micro-nano particle reinforcement |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103769602A (en) * | 2014-01-23 | 2014-05-07 | 聊城大学 | Method for preparing nano-copper/graphene composite particles under assistance of ultrasonic wave |
| CN104479804A (en) * | 2014-11-25 | 2015-04-01 | 华南理工大学 | Nanometer copper/graphene composite material and preparation method and application thereof |
| CN105907444A (en) * | 2016-04-21 | 2016-08-31 | 济宁利特纳米技术有限责任公司 | Additive containing thiadiazole derivative, nano copper and graphene, preparation method of the additive, and lubricant oil containing the additive |
| RU2625453C1 (en) * | 2016-09-21 | 2017-07-14 | федеральное государственное бюджетное образовательное учреждение высшего образования "Донской государственный технический университет",(ДГТУ) | Additive for lubricants |
| CN108531240A (en) * | 2018-04-20 | 2018-09-14 | 厦门六烯科技有限公司 | A kind of graphene-based molybdenum sulfide nano antiwear agent and preparation method thereof |
| CN108531240B (en) * | 2018-04-20 | 2019-04-30 | 厦门六烯科技有限公司 | A kind of graphene-based molybdenum sulfide nano antiwear agent and preparation method thereof |
| CN110624546A (en) * | 2019-10-22 | 2019-12-31 | 特烯（厦门）科技有限公司 | Preparation method of copper/graphene catalyst |
| CN113355146A (en) * | 2021-06-18 | 2021-09-07 | 西安工业大学 | Preparation method of graphene-loaded copper nanoparticles for lubricating oil additive |
| CN114131036A (en) * | 2021-12-03 | 2022-03-04 | 安徽工业大学 | Low-cost preparation method of functionalized micro-nano particle reinforcement |
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Address after: 215500, Suzhou, Jiangsu City, Changshou City province Ho Ho Town Industrial Park Applicant after: The plump sliding material of Jiangsu favour limited-liability company Address before: 215500, Suzhou, Jiangsu City, Changshou City province Ho Ho Town Industrial Park Applicant before: Suzhou Huifeng Lubricant Co., Ltd. |
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Effective date of registration: 20151231 Address after: 215500, Suzhou, Jiangsu Province, Changshou City Tong Town, Ho City Development Zone No. 19 Patentee after: Suzhou Huifeng lubricating material Co., Ltd. Address before: 215500, Suzhou, Jiangsu City, Changshou City province Ho Ho Town Industrial Park Patentee before: The plump sliding material of Jiangsu favour limited-liability company |