CN111243780A - Graphene electric power composite grease - Google Patents
Graphene electric power composite grease Download PDFInfo
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- CN111243780A CN111243780A CN202010176808.0A CN202010176808A CN111243780A CN 111243780 A CN111243780 A CN 111243780A CN 202010176808 A CN202010176808 A CN 202010176808A CN 111243780 A CN111243780 A CN 111243780A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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Abstract
The invention provides graphene electric power composite grease which comprises base grease and a conductive agent, wherein the base grease is 50-100 parts by weight of first ionic liquid, and the conductive agent comprises 0.3-5 parts by weight of ionic liquid modified graphene, 15-50 parts by weight of nano copper powder and 5-20 parts by weight of nano silver powder. The graphene electric power composite grease has good high temperature resistance, low temperature resistance and oxidation resistance, and simultaneously improves the conductivity and the safety.
Description
Technical Field
The invention relates to an electric power composite grease, in particular to an electric power composite grease containing graphene.
Background
The electric composite grease is also called as conductive paste, and is a neutral conductive dressing generally made of base grease, conductive filler, antioxidant stabilizer and the like. The conductive contact surface is widely applied to contact surfaces of the connection positions of buses and buses, buses and equipment wiring terminals and the like in the power industry, and is mainly used for reducing the contact resistance of the conductive contact surface and playing a role in sealing and blocking the contact surface.
The electric composite grease is widely applied to substations, buses and buses in power distribution substations, contact surfaces of joints of the buses and equipment wiring terminals and contact surfaces of isolating switch contacts, and conductors (copper and copper, copper and aluminum, and aluminum) made of the same or different metal materials can be used instead of or better than tin coating and silver coating processes of fastening connection contact surfaces, so that contact resistance can be greatly reduced (35-95 percent can be reduced), temperature rise can be reduced (35-85 percent can be reduced), conductivity of the bus joints and the switch contacts is improved, a large amount of electric energy loss is reduced, various corrosion of the contact surfaces can be avoided, especially, safety performance of the electric composite grease is greatly improved, and reliable guarantee is provided for safe operation of the substations, the power distribution substations and lines.
After the traditional power compound grease runs for a long time, oil bleeding caused by thermal aging, corona aging and the like can occur, and the phenomenon is caused by that molecular chain segments of organic molecular chains in the power compound grease are broken under the condition of heat or corona, so that the molecular weight is reduced, organic grease is separated out, and the electric connection part of power grid equipment is broken.
Therefore, there is a need to develop an electric composite grease material with better aging resistance and stability, and the sealing protection capability of the electric composite grease material on the electric contact part of the power grid equipment is improved.
Disclosure of Invention
The invention aims to provide an electric power composite grease, which is prepared by mixing an ionic liquid serving as a base grease with modified nano metal particles and ionic liquid modified graphene, so that the high temperature resistance, low temperature resistance and oxidation resistance of the electric power composite grease are enhanced, and the electric conductivity and safety are improved.
According to one aspect of the invention, the graphene electric power composite grease comprises base grease and a conductive agent, wherein the base grease is 50-100 parts by weight of ionic liquid, and the conductive agent comprises 0.3-5 parts by weight of ionic liquid modified graphene, 12-40 parts by weight of nano copper powder and 4.5-15 parts by weight of nano silver powder.
Preferably, the ionic liquid includes one or more of a cation selected from the group consisting of a quaternary ammonium salt ion, a quaternary phosphonium salt ion, an imidazolium salt ion, and a pyrrolate salt ion, and an anion selected from the group consisting of a halogen ion, a tetrafluoroborate ion, and a hexafluorophosphate ion.
Preferably, the average particle size of the nano silver powder is 30-500 nm, and the average particle size of the nano copper powder is 15-500 nm.
According to a specific embodiment, the graphene power composite grease further comprises 0.1-1.5 parts by weight of an antioxidant. The antioxidant is preferably thiadiazole or a derivative thereof.
Further, the graphene electric power composite grease also comprises 0.1-5.0 parts by weight of a stabilizer, wherein the stabilizer is citric acid, aromatic amine or phenols.
Further, the ionic liquid electric composite grease also comprises 3.0-8.0 parts by weight of a consistency regulator, wherein the consistency regulator is 8200 or R106.
According to the electric composite grease disclosed by the invention, the ionic liquid is used as the base grease, and the characteristics of the ionic liquid, such as conductivity, difficulty in volatilization, no combustion, large electrochemical stable potential window and the like, are utilized, so that the conductivity of the electric composite grease under the condition of a high electric field is enhanced, the heat productivity of a contact part of power grid equipment is reduced, and meanwhile, the electric grease is difficult to deteriorate in the using process.
Detailed Description
The graphene electric composite grease provided by the invention comprises a base grease and a conductive agent.
Wherein the base grease can be 50-100 parts by weight of the first ionic liquid, preferably room temperature ionic liquid. The first ionic liquid can be formed by combining one or more cations of quaternary ammonium salt ions, quaternary phosphonium salt ions, imidazole salt ions and pyrrole salt ions and one or more of halogen ions, tetrafluoroborate ions and hexafluorophosphate ions.
Preferably, the first ionic liquid may be one or more of tetrafluoroborate imidazolium salts, hexafluorophosphate imidazolium salts, tetrafluoroborate pyrrolium salts, hexafluorophosphate pyrrolium salts, and the like.
The first ionic liquid is used in an amount of 50 to 100 parts by weight, preferably 60 to 90 parts by weight, more preferably 65 to 85 parts by weight, for example 70 parts by weight. If the amount of the ionic liquid is less than 50 parts by weight, the conductive agent particles cannot be sufficiently dispersed, and the system is liable to phase separation and precipitation, so that the stability of the electric composite grease is lowered and the conductivity is lowered. If the ionic liquid is used in an amount of more than 100 parts by weight, the increased amount has a limit to improve the electrical conductivity of the electrical composite grease, but increases the production cost.
The conductive agent may include 0.3 to 5 parts (preferably 1 to 4 parts, and more preferably 1.5 to 3.5 parts) of ionic liquid modified graphene, 15 to 50 parts by weight of nano copper powder, and 5 to 20 parts by weight of nano silver powder. Preferably, the average particle size of the nano silver powder is 30-500 nm, and the average particle size of the nano copper powder is 15-500 nm.
The surface of unmodified graphene is hydrophobic and oleophobic inert, strong van der waals force exists between sheet layers, the graphene is easy to agglomerate, and a good composite system is difficult to form with other matrixes, so that the surface modification is needed.
The ionic liquid modified graphene used in the present invention is graphene modified with a second ionic liquid. Wherein the second ionic liquid may also include a cation selected from the group consisting of a quaternary ammonium salt ion, a quaternary phosphonium salt ion, an imidazolium salt ion, and a pyrrolate salt ion, and an anion selected from the group consisting of a halogen ion, a tetrafluoroborate ion, and a hexafluorophosphate ion. The graphene is preferably 3-10 layers of graphene.
The second ionic liquid may be the same or different from the first ionic liquid, preferably both are the same.
According to a specific embodiment, the method for modifying graphene by using ionic liquid comprises the following steps:
10-30 parts of graphene, 2-15 parts of second ionic liquid and 0.2-0.8 part of silane coupling agent are stirred at a high speed of 1500-2500 r/min for 10-15 min to obtain the ionic liquid modified graphene.
The copper nanoparticles and silver nanoparticles herein are preferably surface-modified to improve their dispersibility in the ionic liquid base grease and dispersion stability, respectively.
The above-mentioned copper nanoparticles and silver nanoparticles may be surface-treated by a method conventional in the art, for example, by a silane coupling agent such as siloxane.
The conventional surface treatment method of the conductive agent powder is as follows: uniformly mixing 20-50 parts by weight of conductive agent powder and 10-15 parts by weight of silane coupling agent to fully soak the powder, then placing the mixed powder in a vacuum oven, treating for 1-4 hours at 100-200 ℃ and a vacuum degree of more than-0.1 MPa, naturally cooling to room temperature, taking out and sealing for later use.
The silane coupling agent may be, for example, one or more of octamethylcyclotetrasiloxane and phenyltriethoxysilane.
According to a specific embodiment, the graphene power complex lipid of the present invention may further include an additive, such as one or more of an antioxidant, a stabilizer, and a consistency regulator.
The antioxidant used in the invention can be thiadiazole or a derivative thereof, and the using amount of the antioxidant can be 0.1-1.5 parts by weight.
The stabilizer used in the present invention may be citric acid, aromatic amine or phenol, and the amount may be 0.1 to 5.0 parts by weight.
The consistency regulator used in the present invention may be white carbon black, such as 8200 or R106, and the amount may be 3.0-8.0 parts by weight.
The graphene electric power composite grease is prepared by adding modified conductive agent powder into ionic liquid according to a required proportion, uniformly mixing, adding an antioxidant, a stabilizer and a consistency regulator, and uniformly grinding.
Above-mentioned graphite alkene electric power composite fat adopts ionic liquid to replace conventional macromolecular resin as basic fat, including ionic liquid modified graphene, nanometer silver powder and nanometer copper powder as the conducting agent powder for ionic liquid modified graphene builds with nanometer metal particle and forms the electrically conductive passageway, is favorable to the improvement of electric conductivity more, and the further reduction of metal contact resistance. On the other hand, the characteristics of high conductivity, low volatility, incombustibility, large electrochemical stable potential window and the like of the ionic liquid and the high conductivity of the modified graphene can be utilized, so that the graphene electric power compound grease disclosed by the invention has obviously enhanced high and low temperature stability and electric conductivity under the condition of a high electric field, the heat productivity of a contact part of power grid equipment can be reduced, the electric power compound grease is prevented from being degraded and deteriorated in the using process, and the defects that organic grease is easy to separate out and deteriorate are overcome.
The graphene electric power composite grease provided by the invention can resist high temperature of more than 300 ℃, the contact resistance change coefficient is less than 0.85, and no dropping point exists.
The technical solutions of the present application will be more clearly illustrated by the following examples.
Examples
Example 1
1. Modification of graphene by tetrafluoroborate imidazolium salt
10g of graphene, 2g of imidazolium tetrafluoroborate and 0.2g of phenyltriethoxysilane are stirred at a high speed for 15min at a stirring speed of 1500r/min to obtain the imidazolium tetrafluoroborate modified graphene.
2. Modification of nano silver powder and nano copper powder
Uniformly mixing 20g of silver powder with the average particle size of 30nm and 10g of silane coupling agent octamethylcyclotetrasiloxane to fully infiltrate the powder, then placing the mixed powder in a vacuum oven, treating for 1 hour at 100 ℃ and a vacuum degree of-0.1 MPa, naturally cooling to room temperature, taking out and sealing for later use.
20g of copper powder with the average particle size of 15nm and 10g of silane coupling agent octamethylcyclotetrasiloxane are uniformly mixed to fully infiltrate the powder, then the mixed powder is placed in a vacuum oven, treated for 1 hour at 100 ℃ and a vacuum degree of-0.1 MPa, naturally cooled to room temperature, taken out and sealed for later use.
3. Preparation of graphene electric power composite grease
3g of the imidazole tetrafluoroborate modified graphene, 45g of the modified nano silver powder and 120g of the modified nano copper powder are added into 500g of ionic liquid imidazole tetrafluoroborate, the mixture is uniformly mixed, and 1g of thiadiazole, 1.2g of citric acid and 30g of white carbon black are added into the mixture and ground for 3 hours to obtain the electric power composite grease.
Example 2
1. Modification of graphene by using hexafluorophosphate imidazolium salt
And stirring 30g of graphene, 15g of imidazole hexafluorophosphate and 0.8g of phenyltriethoxysilane at a stirring speed of 2000r/min at a high speed for 10min to obtain the imidazole hexafluorophosphate modified graphene.
2. Modification of nano silver powder and nano copper powder
50g of silver powder with the average particle size of 200nm and 15g of silane coupling agent octamethylcyclotetrasiloxane are uniformly mixed to fully infiltrate the powder, then the mixed powder is placed in a vacuum oven, treated for 3 hours at 200 ℃ and a vacuum degree of-0.09 MPa, naturally cooled to room temperature, taken out and sealed for later use.
50g of copper powder with the average particle size of 200nm and 15g of silane coupling agent octamethylcyclotetrasiloxane are uniformly mixed to fully infiltrate the powder, then the mixed powder is placed in a vacuum oven, treated for 3 hours at 200 ℃ and a vacuum degree of-0.09 MPa, naturally cooled to room temperature, taken out and sealed for later use.
3. Preparation of graphene electric power composite grease
And adding 50g of imidazole hexafluorophosphate modified graphene, 150g of modified nano silver powder and 400g of modified nano copper powder prepared in the above step into 1000g of ionic liquid imidazole hexafluorophosphate, uniformly mixing, adding 15g of thiadiazole, 50g of citric acid and 80g of white carbon black, and grinding for 3 hours to obtain the electric composite grease.
Example 3
1. Modification of graphene by tetrafluoroborate pyrrolate
Stirring 20g of graphene, 9g of tetrafluoroborate pyrrolate and 0.8g of phenyltriethoxysilane at a stirring speed of 1800r/min at a high speed for 12min to obtain the tetrafluoroborate pyrrolate modified graphene.
2. Modification of nano silver powder and nano copper powder
Uniformly mixing 35g of silver powder with the average particle size of 500nm and 12g of silane coupling agent phenyltriethoxysilane to fully infiltrate the powder, then placing the mixed powder in a vacuum oven, processing for 2 hours at 150 ℃ and a vacuum degree of-0.09 MPa, naturally cooling to room temperature, taking out and sealing for later use.
Uniformly mixing 35g of copper powder with the average particle size of 500nm with 12g of silane coupling agent phenyltriethoxysilane to fully infiltrate the powder, then placing the mixed powder in a vacuum oven, processing for 2 hours at 150 ℃ and a vacuum degree of-0.09 MPa, naturally cooling to room temperature, taking out and sealing for later use.
3. Preparation of graphene electric power composite grease
Adding 25g of tetrafluoroborate pyrrolate modified graphene, 100g of modified nano silver powder and 260g of modified nano copper powder into 750g of ionic liquid tetrafluoroborate pyrrolate, uniformly mixing, adding 10g of thiadiazole, 15g of diphenylamine and 60g of white carbon black, and grinding for 3 hours to obtain the electric power composite grease.
Example 4
1. Modification of graphene by hexafluorophosphate pyrrolate
And stirring 15g of graphene, 6g of hexafluorophosphate pyrrole salt and 0.4g of phenyltriethoxysilane at a stirring speed of 1800r/min at a high speed for 12min to obtain the hexafluorophosphate pyrrole salt modified graphene.
2. Modification of nano silver powder and nano copper powder
Uniformly mixing 35g of silver powder with the average particle size of 300nm and 12g of silane coupling agent phenyltriethoxysilane to fully infiltrate the powder, then placing the mixed powder in a vacuum oven, processing for 2 hours at 150 ℃ and a vacuum degree of-0.09 MPa, naturally cooling to room temperature, taking out and sealing for later use.
Uniformly mixing 35g of copper powder with the average particle size of 300nm and 12g of silane coupling agent phenyltriethoxysilane to fully infiltrate the powder, then placing the mixed powder in a vacuum oven, processing for 2 hours at 150 ℃ and a vacuum degree of-0.09 MPa, naturally cooling to room temperature, taking out and sealing for later use.
3. Preparation of graphene electric power composite grease
Adding 40g of hexafluorophosphate pyrrole salt modified graphene, 120g of modified nano silver powder and 200g of modified nano copper powder into 800g of ionic liquid hexafluorophosphate pyrrole salt, uniformly mixing, adding 10g of thiadiazole, 8g of diphenylamine and 60g of white carbon black, and grinding for 3 hours to obtain the electric power composite grease.
Comparative example 1
45g of modified nano silver powder and 120g of modified nano copper powder prepared according to example 1 are added into 500g of lubricating base oil, the mixture is uniformly mixed, and 1g of thiadiazole, 1.2g of citric acid and 30g of white carbon black are added into the mixture and ground for 3 hours to prepare the electric power composite grease.
Comparative example 2
45g of modified nano silver powder, 120g of modified nano copper powder and 3g of unmodified graphene, which are prepared according to example 1, are added into 500g of lubricating base oil, the mixture is uniformly mixed, and then 1g of thiadiazole, 1.2g of citric acid and 30g of white carbon black are added into the mixture and ground for 3 hours to prepare the electric power composite grease.
Comparative example 3
168g of ionic liquid imidazole tetrafluoroborate is added into 500g of lubricating base oil, the mixture is uniformly mixed, and then 1g of thiadiazole, 1.2g of citric acid and 30g of white carbon black are added into the mixture and ground for 3 hours to prepare the electric power composite grease.
Comparative example 4
45g of ionic liquid imidazole tetrafluoroborate is added into 500g of lubricating base oil, the mixture is uniformly mixed, and then 1g of thiadiazole, 1.2g of citric acid and 30g of white carbon black are added into the mixture and ground for 3 hours to prepare the electric power composite grease.
Performance testing
The performance of the power composite greases prepared according to examples 1 to 4 and comparative examples 1 to 4 were tested according to the following criteria:
cone penetration (25 ℃, 150g) was tested according to GB/T269-1991;
the dropping point was tested according to GB/T3498-1983;
the corrosion resistance was tested according to GB/T7326-1987 (copper, aluminum sheets, 120 ℃, 24 h);
testing the change of the cold contact resistance before and after the electric composite grease coating according to GB/T2423.22-2012;
salt spray test was performed according to SH/T0081-1991 (45# steel sheet, 3 d);
testing the high temperature resistance according to DL/T373-2019;
testing the acceleration stability according to DL/T373-2019;
the test results are shown in table 1 below.
TABLE 1
As can be seen from the results in table 1 above, the graphene power composite greases according to examples 1 to 4 of the present invention have significantly better high-temperature stability and particularly excellent cold contact resistance change coefficient before and after pasting, compared to the power composite greases prepared in comparative documents 1 to 4 using the lubricating base oil as the base grease, the nano silver powder and the nano copper powder as the conductive agent, or the ionic liquid as the conductive agent, and the power composite greases prepared using the ionic liquid as the base grease have no dropping point, which will greatly improve the high-temperature use safety of the power grid device.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
Claims (9)
1. The graphene electric power composite grease is characterized by comprising 50-100 parts by weight of first ionic liquid and a conductive agent, wherein the conductive agent comprises 0.3-5 parts by weight of ionic liquid modified graphene, 12-40 parts by weight of nano copper powder and 4.5-15 parts by weight of nano silver powder.
2. The graphene power complex lipid according to claim 1, the first ionic liquid comprising one or more of a cation selected from a quaternary ammonium salt ion, a quaternary phosphonium salt ion, an imidazolium salt ion, and a pyrrolate salt ion, and an anion selected from a halogen ion, a tetrafluoroborate ion, and a hexafluorophosphate ion.
3. The graphene power complex lipid according to claim 1, the ionic liquid modified graphene being graphene modified with a second ionic liquid comprising one or more of a cation selected from a quaternary ammonium salt ion, a quaternary phosphonium salt ion, an imidazolium salt ion, and a pyrrolate salt ion, and an anion selected from a halogen ion, a tetrafluoroborate ion, and a hexafluorophosphate ion.
4. The graphene electrical composite grease according to claim 1, wherein the average particle size of the copper nanoparticles is 15 to 500 nm.
5. The graphene electrical composite grease according to claim 1, wherein the average particle size of the silver nanoparticles is 30 to 500 nm.
6. The graphene power composite grease according to any one of claims 1 to 5, further comprising 0.1 to 1.5 parts by weight of an antioxidant.
7. The graphene power composite grease according to claim 6, wherein the antioxidant is thiadiazole or a derivative thereof.
8. The graphene electrical composite lipid according to any one of claims 1 to 5, further comprising 0.1 to 5.0 parts by weight of a stabilizer.
9. The ionic liquid electric power composite grease according to any one of claims 1 to 5, further comprising 3.0 to 8.0 parts by weight of a consistency regulator.
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| CN202010176808.0A CN111243780A (en) | 2020-03-13 | 2020-03-13 | Graphene electric power composite grease |
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| CN105255422A (en) * | 2015-11-17 | 2016-01-20 | 张建刚 | Electrically conductive and thermally conductive graphene slurry and preparation method thereof |
| US20170221645A1 (en) * | 2014-08-11 | 2017-08-03 | The Arizona Board Of Regents On Behalf Of The University Of Arizona | Aligned graphene-carbon nanotube porous carbon composite |
| CN108624226A (en) * | 2018-05-25 | 2018-10-09 | 国网江苏省电力有限公司电力科学研究院 | A kind of graphene electric force compounded grease and preparation method thereof |
| CN109354729A (en) * | 2018-07-24 | 2019-02-19 | 黄山市尚义橡塑制品有限公司 | Graphene enhances rubber and preparation method thereof |
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2020
- 2020-03-13 CN CN202010176808.0A patent/CN111243780A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105084348A (en) * | 2014-05-20 | 2015-11-25 | 中国科学院大连化学物理研究所 | Method for preparing conductive graphene dispersion slurry or solid with dispersible water phase |
| US20170221645A1 (en) * | 2014-08-11 | 2017-08-03 | The Arizona Board Of Regents On Behalf Of The University Of Arizona | Aligned graphene-carbon nanotube porous carbon composite |
| CN105255422A (en) * | 2015-11-17 | 2016-01-20 | 张建刚 | Electrically conductive and thermally conductive graphene slurry and preparation method thereof |
| CN108624226A (en) * | 2018-05-25 | 2018-10-09 | 国网江苏省电力有限公司电力科学研究院 | A kind of graphene electric force compounded grease and preparation method thereof |
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Application publication date: 20200605 |