CN117004449A - Preparation method of additive, additive and application of additive in lubricating oil - Google Patents
Preparation method of additive, additive and application of additive in lubricating oil Download PDFInfo
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- CN117004449A CN117004449A CN202310960598.8A CN202310960598A CN117004449A CN 117004449 A CN117004449 A CN 117004449A CN 202310960598 A CN202310960598 A CN 202310960598A CN 117004449 A CN117004449 A CN 117004449A
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- additive
- copper
- hollow sphere
- polypyrrole hollow
- nano polypyrrole
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- 239000000654 additive Substances 0.000 title claims abstract description 71
- 230000000996 additive effect Effects 0.000 title claims abstract description 66
- 239000010687 lubricating oil Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920000128 polypyrrole Polymers 0.000 claims abstract description 65
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000010949 copper Substances 0.000 claims abstract description 37
- 239000002131 composite material Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 32
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052802 copper Inorganic materials 0.000 claims abstract description 27
- 238000000926 separation method Methods 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012286 potassium permanganate Substances 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 150000001879 copper Chemical class 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 10
- 229960004643 cupric oxide Drugs 0.000 claims abstract description 10
- 239000012266 salt solution Substances 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 21
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000000178 monomer Substances 0.000 claims description 15
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 13
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 13
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical group FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 10
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 229960002523 mercuric chloride Drugs 0.000 claims description 10
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 claims description 10
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- UWHVHRVEPWRFSE-UHFFFAOYSA-N mercury 1H-pyrrole Chemical compound [Hg].N1C=CC=C1 UWHVHRVEPWRFSE-UHFFFAOYSA-N 0.000 claims description 8
- 239000003960 organic solvent Substances 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 6
- 230000001590 oxidative effect Effects 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 2
- 239000002199 base oil Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 238000005299 abrasion Methods 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 4
- 238000011161 development Methods 0.000 description 3
- IYWCBYFJFZCCGV-UHFFFAOYSA-N formamide;hydrate Chemical compound O.NC=O IYWCBYFJFZCCGV-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 230000001050 lubricating effect Effects 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 239000002113 nanodiamond Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000005381 potential energy Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/044—Mixtures of base-materials and additives the additives being a mixture of non-macromolecular and macromolecular compounds
-
- 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
- C10M2201/05—Metals; Alloys
-
- 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
- C10M2201/06—Metal compounds
- C10M2201/062—Oxides; Hydroxides; Carbonates or bicarbonates
-
- 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
- C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
- C10M2217/04—Macromolecular compounds from nitrogen-containing monomers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
Landscapes
- 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 application discloses a preparation method of an additive, the additive and application thereof in lubricating oil. The preparation method of the additive comprises the following steps: (1) preparing nano polypyrrole hollow spheres; (2) Adding the nano polypyrrole hollow spheres into copper salt solution, uniformly mixing, adding a reducing agent for reaction, carrying out solid-liquid separation, washing and drying to obtain a nano polypyrrole hollow sphere/copper composite material; (3) Dispersing the nano polypyrrole hollow sphere/copper composite material in water, adding potassium permanganate solution for reaction, performing solid-liquid separation, washing and drying to obtain the additive, wherein the additive is the nano polypyrrole hollow sphere/copper/manganese dioxide composite material. The additive of the application is not only an excellent friction improver, but also can improve the extreme pressure resistance of lubricating oil.
Description
Technical Field
The application relates to the technical field of lubricating oil additives, in particular to a preparation method of an additive, the additive and application of the additive in lubricating oil.
Background
Friction and wear are a phenomenon commonly existing in the nature, and bring economic loss and potential safety hazard to people. And (3) data display: about 33% -50% of the existing energy losses come from frictional wear, more than about 50% of the primary energy is consumed by friction throughout the world, about 60% of machine parts fail due to wear, and wear is one of three main causes of equipment rejection. The economic loss caused by abrasion in China can reach hundreds of billions each year, about 80% of mechanical equipment damage is caused by abrasion of parts, and half of safety production accidents are caused by excessive abrasion and lubrication failure of the equipment. In summary, reducing the frictional wear of mechanical devices is a direction of development by related researchers. The lubrication technology is an important technical measure for improving the friction state of friction pairs, reducing friction resistance and slowing down wear, and the rapid development of the technology is an important way for realizing energy conservation and emission reduction in China and implementing national strategy.
Lubricating oils are used as the auxiliary mechanism for normal operation of engines, and in order to ensure the corresponding performance, auxiliary support of functions by additives is generally adopted in lubricating oils, so that abrasion is further reduced, friction is reduced, and the important value and effect of the performance of the lubricating agents are improved.
In recent years, with development of nanotechnology, research on nano materials as lubricating oil additives is increasingly widespread, nano diamond is used as the lubricating oil additive, and abrasion resistance of lubricating oil is remarkably improved. The nano silicon nitride or nano ferroferric oxide is used as a lubricating oil additive to obtain the anti-oxidation and anti-wear lubricating oil. Graphene has incomparable advantages as a novel nano carbon material, such as good mechanical property, high thermal conductivity and the like, and the special two-dimensional lamellar structure is beneficial to friction reduction, so that the graphene is an ideal lubricating oil additive. However, the compatibility of the graphene and the lubricating oil is poor, and the graphene is easy to agglomerate due to the high surface potential energy, so that the dispersibility of the graphene in the lubricating oil is poor, layering and precipitation are easy to occur, and the performance of the lubricating oil is finally affected.
Thus, there is a need for better performing additives without breaking.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a preparation method of an additive, the additive and application of the additive in lubricating oil. The additive material of the application is nano polypyrrole hollow sphere/copper/manganese dioxide composite material. The additive prepared by the method is used in lubricating base oil to form lubricating oil, so that friction resistance can be effectively reduced, and extreme pressure wear resistance of a lubricating oil film can be fully exerted.
One of the purposes of the application is to provide a preparation method of the additive, which comprises the following steps:
(1) Preparing nano polypyrrole hollow spheres;
(2) Adding the nano polypyrrole hollow spheres into copper salt solution, uniformly mixing, adding a reducing agent for reaction, carrying out solid-liquid separation, washing and drying to obtain a nano polypyrrole hollow sphere/copper composite material;
(3) Dispersing the nano polypyrrole hollow sphere/copper composite material in water, adding potassium permanganate solution for reaction, performing solid-liquid separation, washing and drying to obtain the additive, wherein the additive is the nano polypyrrole hollow sphere/copper/manganese dioxide composite material.
In the method for producing an additive according to the present application, preferably,
in the step (1), the step of (a),
the nano polypyrrole hollow sphere used in the application can be directly purchased or prepared according to the existing method, and the steps for preparing the nano polypyrrole hollow sphere preferably comprise the following steps:
dissolving mercuric chloride in deionized water, adding pyrrole monomers, and uniformly stirring to obtain a solid spherical complex of pyrrole mercuric salt; and then adding an oxidant into the solid spherical complex of the pyrrole mercury salt, and stirring for reaction to obtain the nano polypyrrole hollow sphere.
In the method for producing an additive according to the present application, preferably,
in the step (1), the step of (a),
the oxidant is ammonium persulfate solution;
the feeding mass ratio of the mercuric chloride to the pyrrole monomer is 0.8-1.1:1; and/or the number of the groups of groups,
the feeding mole ratio of the pyrrole monomer to the ammonium persulfate in the oxidant is 1:0.9-1.1.
The diameter of the nano polypyrrole hollow sphere prepared by the method is about 250-350 nanometers.
In the method for producing an additive according to the present application, preferably,
in the step (2), the step of (C),
the concentration of the copper salt solution is 3.5-10 mg/mL;
the copper salt in the copper salt solution is copper sulfate;
the mass ratio of the nano polypyrrole hollow sphere to the copper salt is 1 (8-20);
the solvent of the copper salt solution is a mixed solvent of water and an organic solvent.
In the method for producing an additive according to the present application, preferably,
the volume ratio of water to organic solvent is 1 (1-3);
the organic solvent is DMF.
In the method for producing an additive according to the present application, preferably,
in the step (2), the step of (C),
the reducing agent is sodium hypophosphite solution;
the mass ratio of the sodium hypophosphite to the copper salt is 1 (3-5).
In the method for producing an additive according to the present application, preferably,
in the step (2), the step of (C),
the reaction temperature is 40-50 ℃ and the reaction time is 1-2 hours;
the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 10000-12000 rpm, and the centrifugal time is 15-20 minutes;
the drying temperature is 30-50 ℃ and the drying time is 24-48 hours.
In the method for producing an additive according to the present application, preferably,
in the step (3), the step of (c),
the mass ratio of the nano polypyrrole hollow sphere/copper composite material to the potassium permanganate is 1 (0.1-0.3);
when the nano polypyrrole hollow sphere/copper composite material is dispersed in water, the mass volume ratio of the nano polypyrrole hollow sphere/copper composite material to the water is 1g (100-400 mL); the concentration of the potassium permanganate solution is 1-2 mol/L.
In the method for producing an additive according to the present application, preferably,
in the step (3), the step of (c),
the reaction temperature is room temperature; the reaction time is 2-5 hours;
the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 10000-12000 rpm, and the centrifugal time is 15-20 minutes.
The drying temperature is 30-50 ℃ and the drying time is 24-48 hours.
It is a second object of the present application to provide an additive prepared by the method according to one of the objects of the present application, wherein the additive is a nano polypyrrole hollow sphere/copper/manganese dioxide composite material.
It is a further object of the present application to provide the use of the additive according to the second object of the present application in lubricating oils.
The additive prepared by the method is used in lubricating base oil to form lubricating oil, so that friction resistance can be effectively reduced, and extreme pressure wear resistance of a lubricating oil film can be fully exerted. In the nano polypyrrole hollow sphere/copper/manganese dioxide composite material, copper is firstly loaded inside and outside the nano polypyrrole hollow sphere, then potassium permanganate solution is added to oxidize copper and generate manganese dioxide, so that the manganese dioxide is coated on the outer side of the copper; the three structures possibly have synergistic effect, so that the friction resistance can be effectively reduced, and the extreme pressure wear resistance of the lubricating oil film can be fully exerted.
The endpoints of the ranges and any values disclosed in the present application are not limited to the precise range or value, and the range or value should be understood to include values close to the range or value. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. In the following, the individual technical solutions can in principle be combined with one another to give new technical solutions, which should also be regarded as specifically disclosed herein.
Drawings
FIG. 1 is a plot of the plaque morphology of the additive+base oil (additive to base oil mass ratio of 1:150) oil sample of example 1 of the present application;
figure 2 shows the plaque morphology of the base oil sample.
Detailed Description
The present application is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present application and should not be construed as limiting the scope of the present application, and some insubstantial modifications and adjustments of the present application by those skilled in the art from the present disclosure are still within the scope of the present application.
In addition, the specific features described in the following embodiments may be combined in any suitable manner without contradiction. The various possible combinations of the application are not described in detail in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present application can be made, so long as the concept of the present application is not deviated, and the technical solution formed thereby is a part of the original disclosure of the present specification, and also falls within the protection scope of the present application.
The raw materials used in examples and comparative examples, if not particularly limited, are all as disclosed in the prior art, and are, for example, available directly or prepared according to the preparation methods disclosed in the prior art.
[ example 1 ]
A method for preparing an additive comprising the steps of:
(1) Preparing nano polypyrrole hollow spheres; firstly, dissolving mercuric chloride in deionized water, and adding pyrrole monomers, wherein the feeding mass ratio of the mercuric chloride to the pyrrole monomers is 1:1; uniformly stirring, and reacting for 0.8 hour to obtain a solid spherical pyrrole mercury salt complex; then adding solid spherical pyrrole mercury salt complex into ammonium persulfate solution (the concentration is 0.1 mol/L), and stirring and reacting for 7 hours to obtain nano polypyrrole hollow spheres, wherein the feeding molar ratio of pyrrole monomer to ammonium persulfate is 1:1; the product was centrifuged, washed three times with water and three times with ethanol, and the resulting solid was dried under vacuum at 60℃for 24 hours.
(2) Adding the nano polypyrrole hollow spheres into a copper sulfate solution (5 mg/mL) (the solvent is a mixed solvent of water and DMF (dimethyl formamide) with the volume ratio of 1:2), uniformly mixing, wherein the mass ratio of the nano polypyrrole hollow spheres to the copper sulfate is 1:15, adding a sodium hypophosphite solution (with the concentration of 0.2 mol/L), and reacting for 1.5 hours at 50 ℃, wherein the mass ratio of the sodium hypophosphite to the copper sulfate is 1:4; the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 12000rpm, the centrifugal time is 15 minutes, the washing and drying are carried out, the drying temperature is 50 ℃, and the drying time is 24 hours, thus obtaining the nano polypyrrole hollow sphere/copper composite material;
(3) Dispersing 1g of nano polypyrrole hollow sphere/copper composite material in 300mL of water, adding a potassium permanganate solution (1 mol/L), and reacting for 4 hours at room temperature, wherein the feeding mass ratio of the nano polypyrrole hollow sphere/copper composite material to the potassium permanganate is 1:0.2; the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 12000rpm, the centrifugal time is 20 minutes, the washing and drying are carried out, the drying temperature is 50 ℃, and the drying time is 48 hours, so that the additive is obtained, and the additive is the nano polypyrrole hollow sphere/copper/manganese dioxide composite material.
[ example 2 ]
A method for preparing an additive comprising the steps of:
(1) Preparing nano polypyrrole hollow spheres; firstly, dissolving mercuric chloride in deionized water, and adding pyrrole monomers, wherein the feeding mass ratio of the mercuric chloride to the pyrrole monomers is 0.9:1; uniformly stirring, and reacting for 0.9 hour to obtain a solid spherical pyrrole mercury salt complex; then adding solid spherical complex of pyrrole mercury salt into ammonium persulfate solution (the concentration is 0.1 mol/L), and stirring and reacting for 8 hours to obtain nano polypyrrole hollow spheres, wherein the feeding molar ratio of pyrrole monomer to ammonium persulfate is 1:0.9; the product was centrifuged, washed three times with water and three times with ethanol, and the resulting solid was dried under vacuum at 60℃for 24 hours.
(2) Adding the nano polypyrrole hollow spheres into a copper sulfate solution (3.5 mg/mL) (the solvent is a mixed solvent of water and DMF (dimethyl formamide) with the volume ratio of 1:3), uniformly mixing, wherein the mass ratio of the nano polypyrrole hollow spheres to the copper sulfate is 1:20, adding a sodium hypophosphite solution (with the concentration of 0.2 mol/L), and reacting for 2 hours at the temperature of 40 ℃, wherein the mass ratio of the sodium hypophosphite to the copper sulfate is 1:5; the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 10000rpm, the centrifugal time is 20 minutes, the washing and drying are carried out, the drying temperature is 50 ℃, and the drying time is 48 hours, thus obtaining the nano polypyrrole hollow sphere/copper composite material;
(3) Dispersing 1g of nano polypyrrole hollow sphere/copper composite material in 300mL of water, adding a potassium permanganate solution (2 mol/L), and reacting for 2 hours at room temperature, wherein the feeding mass ratio of the nano polypyrrole hollow sphere/copper composite material to the potassium permanganate is 1:0.3; the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 12000rpm, the centrifugal time is 15 minutes, the washing and drying are carried out, the drying temperature is 50 ℃, and the drying time is 48 hours, so that the additive is obtained, and the additive is a nano polypyrrole hollow sphere/copper/manganese dioxide composite material.
[ example 3 ]
A method for preparing an additive comprising the steps of:
(1) Preparing nano polypyrrole hollow spheres; firstly, dissolving mercuric chloride in deionized water, and adding pyrrole monomers, wherein the feeding mass ratio of the mercuric chloride to the pyrrole monomers is 1:1; uniformly stirring, and reacting for 0.8 hour to obtain a solid spherical pyrrole mercury salt complex; then adding solid spherical pyrrole mercury salt complex into ammonium persulfate solution (the concentration is 0.1 mol/L), and stirring and reacting for 7 hours to obtain nano polypyrrole hollow spheres, wherein the feeding molar ratio of pyrrole monomer to ammonium persulfate is 1:1; the product was centrifuged, washed three times with water and three times with ethanol, and the resulting solid was dried under vacuum at 60℃for 24 hours.
(2) Adding the nano polypyrrole hollow spheres into a copper sulfate solution (10 mg/mL) (the solvent is a mixed solvent of water and DMF (dimethyl formamide), the volume ratio is 1:1), uniformly mixing, wherein the mass ratio of the nano polypyrrole hollow spheres to the copper sulfate is 1:8, and then adding a sodium hypophosphite solution (the concentration is 0.2 mol/L), and reacting for 2 hours at 40 ℃, wherein the mass ratio of the sodium hypophosphite to the copper sulfate is 1:3; the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 12000rpm, the centrifugal time is 20 minutes, the washing and drying are carried out, the drying temperature is 50 ℃, and the drying time is 48 hours, thus obtaining the nano polypyrrole hollow sphere/copper composite material;
(3) Dispersing 1g of nano polypyrrole hollow sphere/copper composite material in 300mL of water, adding potassium permanganate solution (1.2 mol/L), and reacting for 3 hours at room temperature, wherein the feeding mass ratio of the nano polypyrrole hollow sphere/copper composite material to the potassium permanganate is 1:0.2; the solid-liquid separation adopts centrifugal separation, the centrifugal speed is 11000rpm, the centrifugal time is 20 minutes, the washing and drying are carried out, the drying temperature is 50 ℃, and the drying time is 48 hours, so that the additive is obtained, and the additive is a nano polypyrrole hollow sphere/copper/manganese dioxide composite material.
[ example 4 ]
The same preparation method is adopted as in example 1, except that:
the mass ratio of the nano polypyrrole hollow sphere to the copper sulfate is 1:8.
[ example 5 ]
The same preparation method is adopted as in example 1, except that:
the mass ratio of the nano polypyrrole hollow sphere to the copper sulfate is 1:20.
[ example 6 ]
The same preparation method is adopted as in example 1, except that:
the mass ratio of the nano polypyrrole hollow sphere/copper composite material to the potassium permanganate is 1:0.1.
[ example 7 ]
The same preparation method is adopted as in example 1, except that:
the mass ratio of the nano polypyrrole hollow sphere/copper composite material to the potassium permanganate is 1:0.3.
Comparative example 1
The same preparation method is adopted as in example 1, except that:
the method does not comprise the steps (2) and (3), and only the nano polypyrrole hollow sphere is obtained.
Comparative example 2
The same preparation method is adopted as in example 1, except that:
the method does not comprise the step (3) and only obtains the nano polypyrrole hollow sphere/copper composite material.
Comparative example 3
The same preparation method is adopted as in example 1, except that:
in the step (3), nano manganese dioxide particles are directly added and uniformly mixed (purchased from Andi metal materials Co., ltd. In Qing and He county), and the addition amount is the same as the mass of manganese dioxide corresponding to the addition of potassium permanganate in the example 1.
Comparative example 4
The same preparation method is adopted as in example 1, except that:
in the step (3), 1g of nano polypyrrole hollow spheres was dispersed in 300mL of water, and then nano manganese dioxide particles were added and uniformly mixed (purchased from Andi metal materials Co., ltd. In Qinghai county) in the same amount as the mass of manganese dioxide corresponding to the potassium permanganate added in example 1.
The testing method comprises the following steps:
the additives of each example and comparative example were added to base oil and neat base oil for friction performance testing and dispersibility testing, and added to base oil (mineral oil having a viscosity of 30cst at 100 ℃) at a mass ratio of additive to base oil of 1:150, respectively. The test was performed using a MRS-10B four-ball frictional wear tester, and GB/T3142-1982, SH/T0189, SH/T0762 standards were performed. The test results were as follows:
TABLE 1
| Sample of | Coefficient of friction | Diameter of mill spot | Maximum no-bite load | Sintering load |
| Example 1 | 0.055 | 0.293 | 1299 | 2850 |
| Example 2 | 0.068 | 0.335 | 1205 | 2745 |
| Example 3 | 0.062 | 0.315 | 1228 | 2790 |
| Example 4 | 0.060 | 0.313 | 1245 | 2800 |
| Example 5 | 0.065 | 0.327 | 1215 | 2760 |
| Example 6 | 0.063 | 0.316 | 1220 | 2780 |
| Example 7 | 0.058 | 0.309 | 1256 | 2820 |
| Comparative example 1 | 0.13 | 0.584 | 1006 | 2150 |
| Comparative example 2 | 0.083 | 0.475 | 1087 | 2360 |
| Comparative example 3 | 0.075 | 0.432 | 1124 | 2510 |
| Comparative example 4 | 0.091 | 0.487 | 1058 | 2310 |
| Base oil | 0.14 | 0.601 | 960 | 2100 |
The data in Table 1 shows that the friction coefficient and the abrasive spot diameter are greatly reduced after the additive of the application is added into the base oil, and in addition, the maximum seizure-free load and the sintering load are obviously improved relative to the base oil, which indicates that the lubricating oil additive of the application is not only an excellent friction improver, but also can improve the extreme pressure resistance of the lubricating oil.
From the comparison of the grinding spot shapes of fig. 1 and 2, it can also be seen that the lubricating oil additive of the application can reduce the width of grinding marks, reduce the depth of grinding marks, and the grinding marks are clear and uniform, and the surface of the sample block is relatively smooth and the friction and wear degree is light.
The application has been described in detail in connection with the specific embodiments and exemplary examples thereof, but such description is not to be construed as limiting the application. It will be understood by those skilled in the art that various equivalent substitutions, modifications or improvements may be made to the technical solution of the present application and its embodiments without departing from the spirit and scope of the present application, and these fall within the scope of the present application. The scope of the application is defined by the appended claims.
All publications, patent applications, patents, and other references mentioned in this specification are incorporated herein by reference in their entirety. Unless defined otherwise, all technical and scientific terms used herein have the meaning commonly understood by one of ordinary skill in the art. In case of conflict, the present specification, definitions, will control.
When the specification derives materials, substances, methods, steps, devices, or elements and the like in the word "known to those skilled in the art", "prior art", or the like, such derived objects encompass those conventionally used in the art as the application suggests, but also include those which are not currently commonly used but which would become known in the art to be suitable for similar purposes.
In the context of this specification, any matters or matters not mentioned are directly applicable to those known in the art without modification except as explicitly stated.
Claims (10)
1. A method for preparing an additive, comprising the steps of:
(1) Preparing nano polypyrrole hollow spheres;
(2) Adding the nano polypyrrole hollow spheres into copper salt solution, uniformly mixing, adding a reducing agent for reaction, carrying out solid-liquid separation, washing and drying to obtain a nano polypyrrole hollow sphere/copper composite material;
(3) Dispersing the nano polypyrrole hollow sphere/copper composite material in water, adding potassium permanganate solution for reaction, performing solid-liquid separation, washing and drying to obtain the additive, wherein the additive is the nano polypyrrole hollow sphere/copper/manganese dioxide composite material.
2. A process for preparing an additive as claimed in claim 1, wherein,
in the step (1), the step of (a),
the preparation method of the nano polypyrrole hollow sphere comprises the following steps:
dissolving mercuric chloride in deionized water, adding pyrrole monomers, and uniformly stirring to obtain a solid spherical complex of pyrrole mercuric salt; and then adding an oxidant into the solid spherical complex of the pyrrole mercury salt, and stirring for reaction to obtain the nano polypyrrole hollow sphere.
3. The method for preparing the additive according to claim 2, wherein:
in the step (1), the step of (a),
the oxidant is ammonium persulfate solution;
the feeding mass ratio of the mercuric chloride to the pyrrole monomer is 0.8-1.1:1; and/or the number of the groups of groups,
the feeding mole ratio of the pyrrole monomer to the ammonium persulfate in the oxidant is 1:0.9-1.1.
4. The method for preparing the additive according to claim 1, wherein:
in the step (2), the step of (C),
the concentration of the copper salt solution is 3.5-10 mg/mL;
the copper salt in the copper salt solution is copper sulfate;
the mass ratio of the nano polypyrrole hollow sphere to the copper salt is 1 (8-20);
the solvent of the copper salt solution is a mixed solvent of water and an organic solvent;
preferably, the method comprises the steps of,
the volume ratio of water to organic solvent is 1 (1-3);
the organic solvent is DMF.
5. The method for preparing the additive according to claim 1, wherein:
in the step (2), the step of (C),
the reducing agent is sodium hypophosphite solution;
the mass ratio of the sodium hypophosphite to the copper salt is 1 (3-5).
6. The method for preparing the additive according to claim 1, wherein:
in the step (2), the step of (C),
the reaction temperature is 40-50 ℃ and the reaction time is 1-2 hours;
the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 10000-12000 rpm, and the centrifugal time is 15-20 minutes;
the drying temperature is 30-50 ℃ and the drying time is 24-48 hours.
7. The method for preparing the additive according to claim 1, wherein:
in the step (3), the step of (c),
the mass ratio of the nano polypyrrole hollow sphere/copper composite material to the potassium permanganate is 1 (0.1-0.3);
when the nano polypyrrole hollow sphere/copper composite material is dispersed in water, the mass volume ratio of the nano polypyrrole hollow sphere/copper composite material to the water is 1g (100-400 mL);
the concentration of the potassium permanganate solution is 1-2 mol/L.
8. The method for preparing the additive according to claim 1, wherein:
in the step (3), the step of (c),
the reaction temperature is room temperature; the reaction time is 2-5 hours;
the solid-liquid separation adopts centrifugal separation, the centrifugal rotation speed is 10000-12000 rpm, and the centrifugal time is 15-20 minutes;
the drying temperature is 30-50 ℃ and the drying time is 24-48 hours.
9. An additive prepared by the method of any one of claims 1-8, wherein:
the additive is a nano polypyrrole hollow sphere/copper/manganese dioxide composite material.
10. Use of the additive prepared according to the method of claim 9 in lubricating oils.
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