CN117049533B - Method for purifying graphite by electric field induced graphite acid method and application - Google Patents
Method for purifying graphite by electric field induced graphite acid method and application Download PDFInfo
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- CN117049533B CN117049533B CN202311250324.6A CN202311250324A CN117049533B CN 117049533 B CN117049533 B CN 117049533B CN 202311250324 A CN202311250324 A CN 202311250324A CN 117049533 B CN117049533 B CN 117049533B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000010439 graphite Substances 0.000 title claims abstract description 106
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000002253 acid Substances 0.000 title abstract description 10
- 230000005684 electric field Effects 0.000 title abstract description 9
- 239000010687 lubricating oil Substances 0.000 claims abstract description 38
- 239000000654 additive Substances 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 230000000996 additive effect Effects 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 19
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 239000002199 base oil Substances 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000012629 purifying agent Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000000967 suction filtration Methods 0.000 claims abstract description 11
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 62
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 claims description 31
- 239000001263 FEMA 3042 Substances 0.000 claims description 31
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 claims description 31
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 claims description 31
- 229940033123 tannic acid Drugs 0.000 claims description 31
- 235000015523 tannic acid Nutrition 0.000 claims description 31
- 229920002258 tannic acid Polymers 0.000 claims description 31
- 239000011259 mixed solution Substances 0.000 claims description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 21
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 18
- 239000008213 purified water Substances 0.000 claims description 15
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- -1 graphite compound Chemical class 0.000 claims description 12
- 239000007983 Tris buffer Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 7
- 239000003960 organic solvent Substances 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 238000005576 amination reaction Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000000376 reactant Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 2
- 238000000746 purification Methods 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003879 lubricant additive Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Lubricants (AREA)
Abstract
A method for purifying graphite by an electric field induced graphite acid method and application thereof relate to a method for purifying graphite and application thereof. The method for purifying the graphite by using the electric field induced graphite acid method comprises the following steps: placing graphite in a reaction vessel, adding a purifying agent, placing two electrode plates at two ends of the reaction vessel under the conditions of stirring and water bath heating, immersing the two electrode plates in the purifying agent, reacting for a period of time, starting a power supply, reacting for a period of time under the condition that the potential difference of the two electrodes is 36V, and carrying out suction filtration, washing and drying to obtain the high-purity graphite. The high-purity graphite is used for preparing lubricating oil additives. The carbon content of the high-purity graphite prepared by the method is more than 99.99%, so that the method is a purification method for effectively ensuring the fixed carbon of the graphite, and is an effective purification method for purifying the graphite with low granularity and high impurity content. The lubricating oil additive prepared by the invention is added into base oil, and the friction coefficient is reduced to 0.025. The invention can obtain high-purity graphite and lubricating oil additive.
Description
Technical Field
The invention relates to a method for purifying graphite and application thereof.
Background
Graphite is an allotrope of carbon, is a gray black opaque solid, has stable chemical property, is corrosion-resistant, and is not easy to react with agents such as acid, alkali and the like. The carbon dioxide is generated by burning in oxygen, and can be oxidized by strong oxidants such as concentrated nitric acid, potassium permanganate and the like.
Graphite has wide application in the fields of antiwear agents, lubricants, metallurgy, chemical industry, machinery, medical instruments, nuclear energy, automobiles, aerospace and the like as a nonmetallic material with excellent performances of electric conduction, heat conduction, high temperature resistance, corrosion resistance, self-lubricating property and the like.
However, as graphite is increasingly used in the field of high-precision materials, there is an increasing demand for high carbon/high purity graphite. Graphite ores often contain impurities such as Si 2O3、Al2O3、MgO、Fe3O4 and CaO, which are usually present in the form of minerals such as quartz, pyrite, carbonates, and the like. The existing purification methods include an alkali acid method, a hydrofluoric acid method, a chlorine roasting method, a high-temperature roasting method and the like. The alkali acid method equipment is easy to corrode, has high energy consumption, and has the problems of large graphite loss, serious wastewater pollution and the like; hydrofluoric acid is extremely toxic and highly corrosive, so that the environmental protection investment is high; chlorine is toxic and has strong corrosiveness, and has high requirements on equipment operation, so that the chlorine is difficult to popularize and apply; the high temperature method has high equipment cost.
In modern social life, the application and consumption of lubricating oil in various industries are very large, so that the performance of the lubricating oil is key to research by people, and therefore, the lubricating oil additive is urgently required to be matched with the lubricating oil and self-lubricating materials, so that research on the lubricating oil additive becomes an important research hotspot at present. The use of low carbon/low purity graphite as a lubricant oil additive does not enhance antifriction and antiwear effects, and therefore, the need to use high purity graphite and the exploration of the use of high purity graphite to prepare lubricant additives are a problem to be solved by those skilled in the art.
Disclosure of Invention
Aiming at the problems, the invention provides a method for purifying graphite by an electric field induced graphite acid method and application thereof.
The electric field induced graphite acid process purifying process features that the process includes the following steps:
1. Placing graphite in a reaction vessel, adding a purifying agent, placing two electrode plates at two ends of the reaction vessel under the conditions of stirring and water bath heating, immersing the two electrode plates in the purifying agent, and reacting for a period of time;
2. And (3) starting a power supply, reacting for a period of time under the condition that the potential difference of the two electrodes is 36V, then introducing reactants into a suction filtration funnel, washing with purified water under the suction filtration state, and finally drying in an oven to obtain the high-purity graphite.
The high-purity graphite is used for preparing lubricating oil additives.
The high-purity graphite is used for preparing the lubricating oil additive and is prepared by the following steps:
1. Preparation of tannic acid/graphite complex:
Under the ultrasonic condition, dispersing high-purity graphite and tannic acid into absolute ethyl alcohol to obtain a mixed solution; magnetically stirring the mixed solution for a period of time, centrifuging, washing, and freeze-drying to obtain tannic acid/graphite compound;
2. adding lamellar lanthanum oxide into N, N-dimethylformamide, heating to 60-80 ℃, dropwise adding epoxy chloropropane under stirring, stirring at 60-80 ℃ for reacting for 2-4 h, dropwise adding triethylamine, continuously stirring at 60-80 ℃ for reacting for 1-6 h, filtering, washing and drying to obtain amination modified lamellar lanthanum oxide;
3. Dispersing tannic acid/graphite compound and aminated modified lamellar lanthanum oxide into a mixed solution of Tris solution and organic solvent, magnetically stirring for 36-48 h at the reaction temperature of 40-80 ℃, ending the reaction, filtering, washing and drying to obtain the lubricating oil additive.
The principle and the advantages of the invention are as follows:
1. Impurities in the graphite are in adsorption state and free state among graphite particles, are mostly inorganic matters, and are in salt solution in acidic aqueous solution; the salt solution and the graphite can be separated through phase state difference, but the separation effect is limited, and as the graphite surface is adsorbed, the smaller the granularity of the graphite is, the stronger the adsorptivity is, so that the problem of salt adsorption in the graphite must be solved to improve the purity of the graphite; the method has the advantages that under the potential difference of 36V, adsorbed salt is reduced to some extent, the purity is improved to some extent, and compared with no electric field induction, the improvement of graphite fixed carbon is improved from 94.94% to more than 99.99%, so that the method is a purification method for effectively ensuring the graphite fixed carbon, and is an effective purification method for purifying graphite with low granularity and high impurity content;
2. The invention firstly prepares the tannic acid/graphite composite, then carries out amino modification on the lamellar lanthanum oxide, then reacts the tannic acid/graphite composite with the modified lamellar lanthanum oxide, and the amino and tannic acid are crosslinked to increase the sliding of the graphite lamellar and the lanthanum oxide lamellar, thereby having a self-lubricating effect and obviously improving the antifriction and antiwear properties, and the friction coefficient of the base oil added with the lubricating oil additive prepared by the invention is 0.025.
The invention can obtain high-purity graphite and lubricating oil additive.
Detailed Description
The first embodiment is as follows: the method for purifying the graphite by using the electric field induction method in the embodiment is specifically completed by the following steps:
1. Placing graphite in a reaction vessel, adding a purifying agent, placing two electrode plates at two ends of the reaction vessel under the conditions of stirring and water bath heating, immersing the two electrode plates in the purifying agent, and reacting for a period of time;
2. And (3) starting a power supply, reacting for a period of time under the condition that the potential difference of the two electrodes is 36V, then introducing reactants into a suction filtration funnel, washing with purified water under the suction filtration state, and finally drying in an oven to obtain the high-purity graphite.
The second embodiment is as follows: the present embodiment differs from the specific embodiment in that: the purifying agent in the first step is a mixed solution of phosphoric acid, EDTA and purified water. The other steps are the same as in the first embodiment.
And a third specific embodiment: this embodiment differs from the first or second embodiment in that: the volume ratio of the phosphoric acid to the purified water is 1:20, and the concentration of EDTA in the mixed solution of the phosphoric acid, the EDTA and the purified water is 3-5%. The other steps are the same as those of the first or second embodiment.
The specific embodiment IV is as follows: one difference between this embodiment and the first to third embodiments is that: the mass ratio of EDTA to graphite in the first step is 1 (4-6). The other steps are the same as those of the first to third embodiments.
Fifth embodiment: one to four differences between the present embodiment and the specific embodiment are: the reaction time in the first step is 3-4 hours; the temperature of the water bath heating in the first step is 85-95 ℃. Other steps are the same as those of the first to fourth embodiments.
Specific embodiment six: the present embodiment differs from the first to fifth embodiments in that: in the second step, the reaction time is 1.5 h-2 h under the condition that the potential difference of the two electrodes is 36V; in the second step, washing with purified water for 5-10 times in the suction filtration state; the carbon content of the high-purity graphite in the second step is more than 99.99%. Other steps are the same as those of the first to fifth embodiments.
Seventh embodiment: one difference between the present embodiment and the first to sixth embodiments is that: the high-purity graphite is used for preparing lubricating oil additives. Other steps are the same as those of embodiments one to six.
Eighth embodiment: one difference between the present embodiment and the first to seventh embodiments is that: the preparation of the lubricating oil additive by the high-purity graphite is completed according to the following steps:
1. Preparation of tannic acid/graphite complex:
Under the ultrasonic condition, dispersing high-purity graphite and tannic acid into absolute ethyl alcohol to obtain a mixed solution; magnetically stirring the mixed solution for a period of time, centrifuging, washing, and freeze-drying to obtain tannic acid/graphite compound;
2. adding lamellar lanthanum oxide into N, N-dimethylformamide, heating to 60-80 ℃, dropwise adding epoxy chloropropane under stirring, stirring at 60-80 ℃ for reacting for 2-4 h, dropwise adding triethylamine, continuously stirring at 60-80 ℃ for reacting for 1-6 h, filtering, washing and drying to obtain amination modified lamellar lanthanum oxide;
3. Dispersing tannic acid/graphite compound and aminated modified lamellar lanthanum oxide into a mixed solution of Tris solution and organic solvent, magnetically stirring for 36-48 h at the reaction temperature of 40-80 ℃, ending the reaction, filtering, washing and drying to obtain the lubricating oil additive. The other steps are the same as those of embodiments one to seven.
The monolithic lanthanum oxide of this embodiment was prepared according to the method of example one of chinese patent CN108557865A, application No. 201810604184.0.
Detailed description nine: one of the differences between this embodiment and the first to eighth embodiments is: the concentration of the high-purity graphite in the mixed solution in the first step is 6 mg/mL-10 mg/mL; the concentration of tannic acid in the mixed solution in the first step is 5 mg/mL-8 mg/mL; the magnetic stirring time in the first step is 10-12 hours; the volume ratio of the mass of the lamellar lanthanum oxide to the N, N-dimethylformamide in the second step is (2 g-5 g) (25 mL-100 mL); the volume ratio of the mass of the lamellar lanthanum oxide to the epoxy chloropropane in the second step is (2 g-5 g) (25 mL-60 mL); the volume ratio of the mass of the lamellar lanthanum oxide to the triethylamine in the second step is (2 g-5 g) (25 mL-100 mL); the mass ratio of the tannic acid/graphite compound to the amination modified lamellar lanthanum oxide in the third step is 1 (3-5); the volume ratio of the mass of the tannic acid/graphite complex to the Tris solution in the third step is 1mg (2 mL-4 mL); the volume ratio of the Tris solution to the organic solvent in the third step is (2-4 mL) (20-50 mL); the organic solvent in the third step is methanol, ethanol or acetone. Other steps are the same as those of embodiments one to eight.
Detailed description ten: the present embodiment differs from the first to ninth embodiments in that: the lubricating oil additive is uniformly dispersed into the base oil, wherein the lubricating oil additive accounts for 0.1-0.5% of the mass of the base oil. The other steps are the same as those of embodiments one to nine.
The following examples are used to verify the benefits of the present invention:
example 1: the electric field induced graphite acid process purifying process includes the following steps:
1. Placing graphite (fixed carbon is 94.94%) in a reaction container, adding a purifying agent, placing two electrode plates at two ends of the reaction container under the conditions of stirring and water bath heating at 90 ℃, immersing the two electrode plates in the purifying agent, and reacting for 4 hours;
the purifying agent in the first step is a mixed solution of phosphoric Acid (AR), EDTA and purified water; the volume ratio of the phosphoric acid to the purified water is 1:20, and the concentration of EDTA in the mixed solution of the phosphoric acid, the EDTA and the purified water is 4%;
The mass ratio of EDTA to graphite in the first step is 1:5;
2. And (3) starting a power supply, reacting for 2 hours under the condition that the potential difference of the two electrodes is 36V, then introducing reactants into a suction filtration funnel, washing for 10 times by purified water in a suction filtration state, and finally drying in an oven to obtain the high-purity graphite.
The fixed carbon content of the high purity graphite obtained in example 1 was 99.9999%.
Example 2: the preparation of the lubricating oil additive using the high purity graphite obtained in example 1 was accomplished by the following steps:
1. Preparation of tannic acid/graphite complex:
Under the ultrasonic condition, dispersing high-purity graphite (with fixed carbon content of 99.9999%) and tannic acid into absolute ethyl alcohol to obtain a mixed solution; magnetically stirring the mixed solution for 12 hours, centrifugally separating, washing with deionized water for 3 times, and freeze-drying to obtain a tannic acid/graphite compound;
The concentration of the high-purity graphite in the mixed solution in the first step is 10mg/mL;
The concentration of tannic acid in the mixed solution in the first step is 5mg/mL;
2. adding the lamellar lanthanum oxide into N, N-dimethylformamide, heating to 80 ℃, dropwise adding epoxy chloropropane under stirring, stirring at 80 ℃ for reaction for 4 hours, dropwise adding triethylamine, continuously stirring at 80 ℃ for reaction for 5 hours, filtering, washing with deionized water for 3 times, and drying to obtain the amination-modified lamellar lanthanum oxide;
the volume ratio of the mass of the lamellar lanthanum oxide to the N, N-dimethylformamide in the second step is 2g:30mL;
The volume ratio of the mass of the lamellar lanthanum oxide to the epoxy chloropropane in the second step is 2g to 30mL;
The volume ratio of the mass of the lamellar lanthanum oxide to the triethylamine in the second step is 2g to 35mL;
3. Dispersing tannic acid/graphite compound and aminated modified lamellar lanthanum oxide into a mixed solution of Tris solution and absolute ethyl alcohol, magnetically stirring for 42h at a reaction temperature of 60 ℃, filtering, washing with deionized water for 3 times, and drying to obtain a lubricating oil additive;
the mass ratio of the tannic acid/graphite compound to the amination modified lamellar lanthanum oxide in the third step is 1:4;
the volume ratio of the mass of the tannic acid/graphite complex to the Tris solution in the third step is 1 mg/3 mL;
The volume ratio of the Tris solution to the absolute ethyl alcohol in the step three is 3mL to 50mL.
The high-purity graphite (fixed carbon content is 99.9999%) prepared in example 1 was dispersed in base oil 250N, the high-purity graphite accounting for 0.1% by mass of the base oil, and this lubricating oil was designated as lubricating oil a;
the lubricating oil additive prepared in example 2 was dispersed in base oil 250N, the mass fraction of the lubricating oil additive was 0.1% of the base oil, and this lubricating oil was designated lubricating oil B;
Graphite having 94.94% of fixed carbon was dispersed in the base oil 250N, and the graphite having 94.94% of fixed carbon was 0.1% by mass of the base oil, which was designated as lubricating oil C.
The lubrication performance of the base oil 250N, the lubricating oil A, the lubricating oil B and the lubricating oil C is researched by adopting a four-ball friction tester; all friction tests were carried out at standard temperature, load 392N and rotational speed 1200r/min for 1 hour; the steel ball used in the experiment is GCr15 bearing steel with the diameter of 12.7mm, the hardness is 61-65HRC, and the abrasion resistance is shown in Table 1;
TABLE 1
| Oil sample | Coefficient of friction |
| Base oil 250N | 0.097 |
| Lubricating oil A | 0.064 |
| Lubricating oil B | 0.025 |
| Lubricating oil C | 0.086 |
As can be seen from table 1: the high-purity graphite and the lubricating oil additive prepared by the invention have excellent lubricating performance. The invention firstly prepares the tannic acid/graphite composite, then carries out amino modification on the lamellar lanthanum oxide, then reacts the tannic acid/graphite composite with the modified lamellar lanthanum oxide, and the amino and tannic acid are crosslinked to increase the sliding of the graphite lamellar and the lanthanum oxide lamellar, thereby improving the self-lubricating effect and the antifriction and antiwear performance obviously.
Claims (8)
1. The application of the high-purity graphite is characterized in that the high-purity graphite is used for preparing lubricating oil additives, and is specifically completed according to the following steps:
1. Preparation of tannic acid/graphite complex:
Under the ultrasonic condition, dispersing high-purity graphite and tannic acid into absolute ethyl alcohol to obtain a mixed solution; magnetically stirring the mixed solution for a period of time, centrifuging, washing, and freeze-drying to obtain tannic acid/graphite compound;
2. Adding the lamellar lanthanum oxide into N, N-dimethylformamide, heating to 60-80 ℃, dropwise adding epoxy chloropropane under the stirring condition, stirring at 60-80 ℃ for reaction for 2-4 hours, dropwise adding triethylamine, continuously stirring at 60-80 ℃ for reaction for 1-6 hours, filtering, washing and drying to obtain the amination modified lamellar lanthanum oxide;
3. Dispersing tannic acid/graphite compound and aminated modified lamellar lanthanum oxide into a mixed solution of Tris solution and organic solvent, magnetically stirring at the reaction temperature of 40-80 ℃ for 36-48 hours, and after the reaction, filtering, washing and drying to obtain a lubricating oil additive;
The concentration of the high-purity graphite in the mixed solution in the first step is 6 mg/mL-10 mg/mL; the concentration of tannic acid in the mixed solution in the first step is 5 mg/mL-8 mg/mL; the magnetic stirring time in the first step is 10-12 hours; the volume ratio of the mass of the lamellar lanthanum oxide to the N, N-dimethylformamide in the second step is (2 g-5 g) (25 mL-100 mL); the volume ratio of the mass of the lamellar lanthanum oxide to the epoxy chloropropane in the second step is (2 g-5 g) (25 mL-60 mL); the volume ratio of the mass of the lamellar lanthanum oxide to the triethylamine in the second step is (2 g-5 g) (25 mL-100 mL); the mass ratio of the tannic acid/graphite compound to the amination modified lamellar lanthanum oxide in the third step is 1 (3-5); the volume ratio of the mass of the tannic acid/graphite complex to the Tris solution in the third step is 1mg (2 mL-4 mL); the volume ratio of the Tris solution to the organic solvent in the third step is (2 mL-4 mL) (20 mL-50 mL); the organic solvent in the third step is methanol, ethanol or acetone.
2. The use of high purity graphite according to claim 1, characterized in that the method is specifically carried out by the following steps:
1. Placing graphite in a reaction vessel, adding a purifying agent, placing two electrode plates at two ends of the reaction vessel under the conditions of stirring and water bath heating, immersing the two electrode plates in the purifying agent, and reacting for a period of time;
2. And (3) starting a power supply, reacting for a period of time under the condition that the potential difference of the two electrodes is 36V, then introducing reactants into a suction filtration funnel, washing with purified water under the suction filtration state, and finally drying in an oven to obtain the high-purity graphite.
3. The use of high purity graphite according to claim 2, wherein the purifying agent in step one is a mixture of phosphoric acid, EDTA and purified water.
4. The use of the high purity graphite according to claim 3, wherein the volume ratio of phosphoric acid to purified water is 1:20, and the concentration of EDTA in the mixture of phosphoric acid, EDTA and purified water is 3% -5%.
5. The use of high purity graphite according to claim 3, wherein the mass ratio of EDTA to graphite in step one is 1 (4-6).
6. The use of high purity graphite according to claim 2, wherein the reaction time in step one is 3-4 hours; the water bath heating temperature in the first step is 85-95 ℃.
7. The use of high purity graphite according to claim 2, wherein the reaction time in step two is 1.5h to 2h at a potential difference of 36V between the electrodes; in the second step, washing with purified water for 5-10 times in a suction filtration state; the fixed carbon content of the high-purity graphite in the second step is more than 99.99%.
8. The application of the high-purity graphite according to claim 1, wherein the lubricating oil additive is uniformly dispersed in the base oil, and the lubricating oil additive accounts for 0.1-0.5% of the base oil by mass.
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