CN116590071A - Poly-zwitterionic carbon dot water lubricating additive and application thereof - Google Patents
Poly-zwitterionic carbon dot water lubricating additive and application thereof Download PDFInfo
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- CN116590071A CN116590071A CN202310377107.7A CN202310377107A CN116590071A CN 116590071 A CN116590071 A CN 116590071A CN 202310377107 A CN202310377107 A CN 202310377107A CN 116590071 A CN116590071 A CN 116590071A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000000654 additive Substances 0.000 title claims abstract description 18
- 230000000996 additive effect Effects 0.000 title claims abstract description 16
- 230000001050 lubricating effect Effects 0.000 title claims abstract description 16
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 17
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 claims abstract description 13
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 11
- 239000008103 glucose Substances 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 8
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000004108 freeze drying Methods 0.000 claims abstract description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 239000000725 suspension Substances 0.000 claims description 19
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 10
- 238000005461 lubrication Methods 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- 238000000502 dialysis Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 2
- 229920002463 poly(p-dioxanone) polymer Polymers 0.000 claims 6
- 239000000622 polydioxanone Substances 0.000 claims 6
- 239000003879 lubricant additive Substances 0.000 claims 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 11
- 239000000047 product Substances 0.000 abstract description 11
- 239000006185 dispersion Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 5
- 230000036571 hydration Effects 0.000 abstract description 5
- 238000006703 hydration reaction Methods 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 238000007142 ring opening reaction Methods 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000003607 modifier Substances 0.000 abstract 1
- 238000012986 modification Methods 0.000 description 11
- 230000004048 modification Effects 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 10
- 238000005299 abrasion Methods 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 7
- -1 polytetrafluoroethylene Polymers 0.000 description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- 239000006228 supernatant Substances 0.000 description 5
- 238000003763 carbonization Methods 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 230000001603 reducing effect Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/64—Environmental friendly compositions
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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 provides a polydirectional ionized carbon dot water lubricating additive and application thereof, belonging to the technical field of new materials. The additive is prepared by the following method: glucose is used as a carbon source, polyethyleneimine is used as a modifier, two substances are dissolved and then react with high temperature heating in a sealed container, the reaction product is cooled to room temperature, and then the nitrogen-doped carbon point is obtained by filtering and evaporating the solvent; dispersing nitrogen-doped carbon points in a solvent, dropwise adding 1,3 propane sultone in an oil bath environment at 30-40 ℃, continuously stirring for 3-5 hours to obtain a precipitate, cleaning the precipitate, ultrasonically dissolving, dialyzing the obtained solution, and freeze-drying to obtain a target product. The invention adopts simple and controllable ring-opening reaction to graft hydrophilic amphoteric ion on the surface of nitrogen doped carbon point, the hydration of the amphoteric ion group endows the carbon point with good dispersibility and lubricity in water, and the water lubricating additive has long dispersion stability exceeding 90 days in water and has excellent antiwear and antifriction effects on metal/metal friction pairs.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a water-dispersible polydiionic carbon dot water lubrication additive and application thereof.
Background
Water is a lubricant with high cooling capacity and low cost, and is widely applied to industrial occasions. However, water cannot be used as a high-efficiency lubricant due to the defects of poor bearing, low viscosity, easy corrosion and the like, so that the preparation of a proper hydrophilic additive plays an indispensable role in water lubrication, so as to improve the lubricating performance of water, exert the environmental protection advantage of water and expand the application field of the water.
The carbon dots have the excellent performances of small size, low precursor cost, designable surface and the like, and can be used as a lubricating additive to be well embedded into a friction interface to play a good role in polishing, repairing and converting sliding friction into rolling friction. Nitrogen is considered an iron-based "active element" and is effective in reducing friction, wear and corrosion. The nitrogen doping can not only improve the hydrophilicity of the carbon material, but also provide rich reaction sites for further functional modification.
The single nitrogen-doped carbon point has the carbon core as a support, and the surface of the carbon core has a large amount of amino groups, so that the carbon core has better bearing capacity, has obviously improved performances such as wear resistance, antifriction and the like compared with water, and still has a larger lifting space.
Disclosure of Invention
In order to solve at least one of the problems, the invention aims to provide the water lubrication additive for the nitrogen-doped carbon dots, which is characterized in that the carbon dots are modified functionally by the zwitterions to play a role in synergistic lubrication of a carbon core and zwitterions, meanwhile, the charged groups of the zwitterions can be combined with surrounding water molecules to form a hydration layer surrounding charges in an aqueous medium, the hydration layer can improve the dispersibility of the nano-additive in water and slow down the inherent agglomeration phenomenon of the nano-additive in water, the problems of the dispersion stability and the agglomeration of the carbon dots in water are solved, and the hydration capability of the carbon dots is improved, so that the water-dispersible poly-zwitterionic carbon dots are obtained.
In order to achieve the above object, the technical scheme of the present invention is as follows:
a polydirectional ionized carbon point water lubrication additive, which is prepared by adopting a method comprising the following steps of;
preparation of nitrogen-doped carbon dots using polyethylenimine and glucose: taking polyethyleneimine and glucose in anhydrous monohydric alcohol to form suspension; and (3) placing the suspension into a sealed reaction kettle, heating for 10-15 hours at 160-200 ℃, filtering the reaction product, and evaporating the solvent to obtain the nitrogen-doped carbon dots.
In the step, the reaction kettle is selected from reaction kettles which do not react with raw materials and products, such as a polytetrafluoroethylene reaction kettle.
In the step, polyethyleneimine with rich amino groups on the surface is selected for carbon doping, and the proportion of polyethyleneimine to glucose is not too high in specific operation, so that crosslinking is caused by too high proportion; too low a ratio may result in incomplete nitrogen doping at the surface of the carbon dots. Too high a ratio of polyethylenimine to anhydrous monohydric alcohol can cause increase of solution viscosity, resulting in uneven carbon source distribution in the mixed solution, which is unfavorable for nitrogen doping process; too low a ratio may result in too low a yield in the nitrogen doping process, resulting in an undoped portion of the finished product. Therefore, through a large number of experiments by the inventor, the proportion of the polyethylenimine and the anhydrous monohydric alcohol is in the range of 10-20 mg/ml, and the mass ratio of the polyethylenimine to the glucose is 1: (1-4) the best results are obtained.
As for the carbonization process, a great number of experiments by the inventor show that the carbonization agent has better effect when the temperature is 160-200 ℃ and the time is 10-15 hours. Too high a temperature and too long a time can lead to excessive carbonization and reduced water dispersibility; too low a temperature and a short time can lead to incomplete carbonization, and the carbon nuclei are smaller and the yield is lower, preferably the temperature is 180 ℃ and the time is 12 hours.
The polyethyleneimine is one of molecular weights 10000, 1800 and 600.
Preparing a polyamphoterion carbon dot by adopting a nitrogen-doped carbon dot: dispersing nitrogen doped carbon dots in anhydrous monohydric alcohol, dropwise adding zwitterionic 1,3 propane sultone at the reaction temperature of 30-40 ℃, continuously stirring for 3-5 hours to obtain a precipitate, adding the precipitate into the anhydrous monohydric alcohol for cleaning, then adding ionized water, and performing ultrasonic dissolution to obtain a polyammonium carbon dot solution, wherein the zwitterionic in the just reacted polyammonium carbon dot aqueous solution has been successfully grafted, the aqueous solution has good lubricating performance, but contains impurities, the addition amount of effective substances is inconvenient to control when the industrial use is carried out, so that the purification operation can be increased, the carbon dot solution is dialyzed for 3-6 days, and freeze-dried to obtain the polyammonium carbon dot powder; wherein each 1-2 g of nitrogen doped carbon point corresponds to 3-6 ml of 1,3 propane sultone.
In the step, the reaction temperature is controlled to be 30-40 ℃, and the temperature can be controlled by means of water bath, oil bath and the like during specific operation.
Dispersing nitrogen-doped carbon points in anhydrous monohydric alcohol, and dropwise adding amphoteric ions 1,3 propane sultone into the anhydrous monohydric alcohol, wherein if the addition amount of the 1,3 propane sultone is small and the reaction time is short, the ring-opening reaction is incomplete, so that the grafting rate of the amphoteric ions on the surface of the nitrogen-doped carbon points is too low; if the addition amount is too large and the reaction time is long, the time cost is increased, and waste is caused. Thus, through extensive experiments by the inventors, it was found that 5ml of 1,3 propane sultone is preferable for every 1 to 2g of nitrogen-doped carbon dots, and the reaction time is 4 hours. After the reaction-completed precipitate was taken out, the precipitate was washed with anhydrous monohydric alcohol several times until the supernatant was colorless and transparent in order to remove the residual solvent therefrom.
In the above steps, the anhydrous monohydric alcohol may be common water-soluble monohydric alcohol such as anhydrous ethanol and anhydrous methanol.
Another object of the present invention is to provide the use of the above water-dispersible poly-zwitterionic carbon spot as a water-lubricating additive, wherein the addition amount thereof is 0.1 to 2.0% by mass of water.
The beneficial effects are that: according to the invention, a simple and controllable ring-opening reaction is adopted to graft hydrophilic amphoteric ions on the surface of the nitrogen-doped carbon dot, and the hydration of the zwitterionic groups endows the poly-zwitterionic carbon dot with good dispersibility and lubricating property in water, so that the long-term dispersion stability of the poly-zwitterionic carbon dot in water exceeding 90 days is easily realized. The prepared polydirectional ionized carbon dots can be directly dispersed into water, have good lubricating effect, and have excellent anti-wear and antifriction effects on metal/metal friction pairs.
Drawings
FIG. 1 is a TEM profile of the product of example 1, wherein FIG. 1a is a TEM profile of nitrogen-doped carbon dots before modification and FIG. 1b is a TEM profile of poly-zwitterionic carbon dots after modification;
FIG. 2 is a graph of XPS scan results for the product of example 1;
FIG. 3 is a graph showing the friction coefficient curves of the products, wherein FIG. 3a is a graph showing the friction coefficient curves of examples 1, 2, 3, 4, water and nitrogen doped carbon points, and FIG. 3b is a graph showing the friction coefficient curves of different concentrations of example 1;
FIG. 4 is a graph of the wear results for water and the product of example 1 at optimum concentration, wherein FIG. 4a is a wear profile, FIG. 4b is a wear 2D plan view, and FIG. 4c is a wear 3D perspective view;
FIG. 5 is a graph showing the dispersion stability of nitrogen-doped carbon dots and polyamphoionized carbon dots in example 1.
Detailed Description
The following detailed description of the invention will be clearly and fully described in connection with the examples which are set forth to illustrate, but are not necessarily all embodiments of the invention.
The percentages in this example are mass percentages unless otherwise indicated.
The invention is further described below with reference to examples:
the following detailed description of the invention will be clearly and fully described in connection with the examples which are set forth to illustrate, but are not necessarily all embodiments of the invention.
The invention is further described below with reference to examples:
in the following examples, unless otherwise specified, the operations described are conventional in the art.
In the examples described below, the starting materials employed are all commercially available, unless otherwise specified.
Example 1
Preparation of nitrogen-doped carbon dots
Taking 1g of polyethyleneimine with molecular weight of 10000 and 2g of glucose in 50ml of absolute ethyl alcohol to form suspension, placing the suspension in a sealed polytetrafluoroethylene reaction kettle, heating the suspension for 12 hours at 180 ℃, cooling the suspension to room temperature, filtering the reaction product, and evaporating the solvent to obtain nitrogen-doped carbon dots.
Preparation of a Polyzwitterionic carbon dot
Dispersing 1g of nitrogen-doped carbon point in 30ml of absolute ethyl alcohol, slowly dripping 5ml of zwitterionic 1,3 propane sultone in an oil bath environment at 35 ℃, and continuously stirring for 4 hours to obtain a precipitate; the precipitate was washed with absolute ethanol until the supernatant was colorless and transparent. Then deionized water is added, ultrasonic dissolution is carried out, the obtained solution is dialyzed for 5 days (the molecular weight cut-off of a dialysis bag is 3500 Da), and the polyamphoterion carbon dot powder is obtained through freeze drying.
Example 2
Preparation of nitrogen-doped carbon dots
Taking 0.5g of polyethyleneimine with the molecular weight of 1800 and 2g of glucose in 50ml of absolute methanol to form suspension, placing the suspension in a sealed polytetrafluoroethylene reaction kettle, heating the suspension for 15h at 160 ℃, filtering the reaction product, and evaporating the solvent to obtain the nitrogen-doped carbon dots.
Preparation of a Polyzwitterionic carbon dot
Dispersing 1g of nitrogen-doped carbon point in 20ml of absolute methanol, slowly dropwise adding 3ml of zwitterionic 1,3 propane sultone in an oil bath environment at 40 ℃, and continuously stirring for 3 hours to obtain a precipitate; the precipitate was washed with anhydrous methanol until the supernatant was colorless and transparent, then deionized water was added, and the resulting solution was sonicated, dialyzed for 4 days (dialysis bag cut-off molecular weight 3500 Da), and freeze-dried to obtain a polyamphoterion carbon dot powder.
Example 3
Preparation of nitrogen-doped carbon dots
Taking 1g of polyethyleneimine with molecular weight of 600 and 1g of glucose in 50ml of absolute ethyl alcohol to form suspension, placing the suspension in a sealed polytetrafluoroethylene reaction kettle, heating the suspension for 10 hours at 200 ℃, cooling the suspension to room temperature, filtering a reaction product, and evaporating a solvent to obtain a nitrogen-doped carbon point.
Preparation of a Polyzwitterionic carbon dot
Dispersing 1g of nitrogen-doped carbon point in 30ml of absolute ethyl alcohol, slowly dripping 6ml of zwitterionic 1,3 propane sultone in an oil bath environment at 30 ℃, and continuously stirring for 5 hours to obtain a precipitate; washing the precipitate with absolute ethanol until the supernatant is colorless and transparent, adding deionized water, dissolving with ultrasound, dialyzing the obtained solution for 6 days (dialysis bag with molecular weight cutoff of 3500 Da), and lyophilizing to obtain the polyamphoterion carbon dot powder.
Example 4
Taking 1g of polyethyleneimine with molecular weight of 10000 and 5g of glucose in 50ml of absolute ethyl alcohol to form suspension, placing the suspension in a sealed polytetrafluoroethylene reaction kettle, heating the suspension for 12 hours at 160 ℃, cooling the suspension to room temperature, filtering the reaction product, and evaporating the solvent to obtain nitrogen-doped carbon dots.
Preparation of a Polyzwitterionic carbon dot
Dispersing 1g of nitrogen-doped carbon point in 30ml of absolute ethyl alcohol, slowly dripping 5ml of zwitterionic 1,3 propane sultone in an oil bath environment at 35 ℃, and continuously stirring for 4 hours to obtain a precipitate; the precipitate was washed with absolute ethanol until the supernatant was colorless and transparent. Then deionized water is added, ultrasonic dissolution is carried out, the obtained solution is dialyzed for 5 days (the molecular weight cut-off of a dialysis bag is 3500 Da), and the polyamphoterion carbon dot powder is obtained through freeze drying.
To further illustrate the effect of the present invention, specific tests were performed on the water-dispersible poly (zwitterionic) carbon dots of the above examples.
1. TEM analysis
The product of example 1 was taken for TEM analysis and the final results are shown in figure 1. Wherein fig. 1a is a TEM topography of nitrogen-doped carbon dots before modification, and fig. 1b is a TEM topography of the polyamphoionized carbon dots. As can be seen from fig. 1, the shape of the spherical nano particles before modification is monodisperse, and the average particle diameter is 3.08nm; the shape of the modified spherical nano particles is still monodisperse, the spherical nano particles are basically unchanged, the average particle size is 3.32nm, the modification process is not obviously destroyed to the morphology, and the success of modification is reflected due to the increase of the particle size.
2. XPS analysis
The product of example 1 was taken for XPS analysis, and the final result is shown in fig. 2, where it can be seen from fig. 2 that the nitrogen-doped carbon dot nanoparticles are mainly composed of C, N and O elements before modification, and the poly-zwitterionic carbon dot nanoparticles also detected S element after modification, indicating that the zwitterionic 1,3 propane sultone was successfully grafted to the nitrogen-doped carbon dot surface.
3. Antiwear antifriction performance test
The lubricating liquid is formed by adding the products prepared in examples 1, 2, 3 and 4 into water for dispersion, the lubricating performance of a steel/steel friction pair is tested in a reciprocating friction mode, the test load is 30N, the frequency is 2HZ, the specific result is shown in figure 3a, the friction coefficient of the added lubricating liquid is greatly reduced compared with that of water, and the result shows that the water-dispersible poly-amphoteric ionized carbon dot nano particles can have excellent antifriction effect, and the performance is poor under the same concentration due to incomplete nitrogen doping caused by the fact that the proportion of polyethylenimine to glucose is too low as shown in example 4. Referring to FIG. 3b, the friction reducing properties of the additive are best at an addition level of 1.5 wt%. Meanwhile, referring to the abrasion sectional view of fig. 4a, the abrasion area of the lubricating liquid is obviously reduced compared with the abrasion area of water, and the abrasion mark surface is smoother and smoother after the lubricating liquid is added through the abrasion 2D plan view of fig. 4b and the abrasion 3D perspective view of fig. 4c, so that the abrasion resistance of the water can be effectively improved after the product of the embodiment 1 is added. The coefficient of friction and wear volume were reduced by 72.5% and 66.1% with respect to water, respectively, with the addition of the lubricating fluid of example 1.
4. Dispersion stability test
The dispersion stability of nanoparticles in water is a critical factor in their performance in water lubrication. The nitrogen-doped carbon dots and the polyamphoionized carbon dots in example 1 were taken separately, added to water in an amount of 0.5wt%, and then left for a while, and the dispersibility of the aqueous solution was observed for various periods of time. The final results are shown in FIG. 5, and the water-dispersible nitrogen-doped carbon dots and the water-dispersible polyzwitterionic carbon dots prepared in the embodiment of the invention are still clear and have no precipitation after being added into water for 90 days, and show excellent dispersion stability.
The present invention has been disclosed in the foregoing description of preferred embodiments, but it will be understood by those skilled in the art that these embodiments are merely for the purpose of describing the present invention and should not be construed as limiting the scope of the present invention. Further modifications are possible without departing from the principles of the invention, and such modifications should be considered as protecting the invention.
Claims (6)
1. The polydirectional ionized carbon point water lubricating additive is characterized by being prepared by a method comprising the following steps of;
(1) Adding polyethylenimine and glucose with the mass ratio of 1:1-1:4 into anhydrous monohydric alcohol to form suspension, wherein the proportion of polyethylenimine to anhydrous monohydric alcohol is 10-20 mg/ml;
(2) Placing the suspension into a sealed reaction kettle, heating for 10-15 h at 160-200 ℃, filtering the reaction product, and evaporating the solvent to obtain a nitrogen-doped carbon point;
(3) Dispersing nitrogen-doped carbon points in anhydrous monohydric alcohol, dropwise adding 1,3 propane sultone at the reaction temperature of 30-40 ℃, and continuously stirring for 3-5 hours to obtain precipitate, wherein 3-6 ml of 1,3 propane sultone is correspondingly added to each 1-2 g of nitrogen-doped carbon points;
(4) And (3) washing the precipitate in the step (3) with anhydrous monohydric alcohol, then adding deionized water, and performing ultrasonic dissolution to obtain the water solution of the polydioxanone carbon dots.
2. The polydioxanone carbon dot water lubricant additive of claim 1, wherein the anhydrous monohydric alcohol is at least one of anhydrous methanol and anhydrous ethanol.
3. The polydioxanone carbon dot water lubricant additive of claim 1, wherein the polyethyleneimine has a molecular weight of any one of 10000, 1800, 600.
4. A polydioxanone carbon dot water-lubricating additive according to any one of claims 1 to 3, characterized in that the preparation process further comprises dialyzing the obtained aqueous solution for 3 to 6 days, and freeze-drying to obtain a polydioxanone carbon dot powder.
5. The polydioxanone carbon dot water lubrication additive of claim 4, wherein the dialysis bag cutoff molecular weight is 3500Da during dialysis.
6. Use of a polyamphoenized carbon dot according to claim 5 as a water lubrication additive, wherein the addition amount thereof is 0.1 to 2.0% by mass of water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310377107.7A CN116590071B (en) | 2023-04-11 | 2023-04-11 | Poly-zwitterionic carbon dot water lubricating additive and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN202310377107.7A CN116590071B (en) | 2023-04-11 | 2023-04-11 | Poly-zwitterionic carbon dot water lubricating additive and application thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20140027677A1 (en) * | 2011-03-15 | 2014-01-30 | University Of Kentucky Research Foundation | Carbon particles |
| CN108455564A (en) * | 2018-02-05 | 2018-08-28 | 中南民族大学 | A method of preparing yellow or green carbon dots |
| CN111944586A (en) * | 2020-08-26 | 2020-11-17 | 合肥工业大学 | Metal processing water lubricating nano additive and preparation method thereof |
| CN114703003A (en) * | 2022-04-14 | 2022-07-05 | 上海绿晟环保科技有限公司 | Carbon quantum dot-loaded nano-material lubricating additive and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140027677A1 (en) * | 2011-03-15 | 2014-01-30 | University Of Kentucky Research Foundation | Carbon particles |
| CN108455564A (en) * | 2018-02-05 | 2018-08-28 | 中南民族大学 | A method of preparing yellow or green carbon dots |
| CN111944586A (en) * | 2020-08-26 | 2020-11-17 | 合肥工业大学 | Metal processing water lubricating nano additive and preparation method thereof |
| CN114703003A (en) * | 2022-04-14 | 2022-07-05 | 上海绿晟环保科技有限公司 | Carbon quantum dot-loaded nano-material lubricating additive and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 路晨;余莉萍;: "超支化聚乙烯亚胺改性荧光碳点材料的制备和表征", 化学工业与工程, vol. 36, no. 03, 3 July 2018 (2018-07-03), pages 16 - 21 * |
| 车望远;刘长军;杨焜;李钒;杨伟文;田丰;: "荧光碳点的制备和性质及其应用研究进展", 复合材料学报, vol. 33, no. 03, 31 March 2016 (2016-03-31), pages 431 - 450 * |
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