CN107880972A - A kind of preparation method of lubricating oil composite Nano antiwear additive - Google Patents

A kind of preparation method of lubricating oil composite Nano antiwear additive Download PDF

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CN107880972A
CN107880972A CN201711033815.XA CN201711033815A CN107880972A CN 107880972 A CN107880972 A CN 107880972A CN 201711033815 A CN201711033815 A CN 201711033815A CN 107880972 A CN107880972 A CN 107880972A
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lubricating oil
preparation
antiwear additive
composite nano
nano
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CN107880972B (en
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汪涛
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Tangshan Cheng You Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/02Carbon; Graphite
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/10Metal oxides, hydroxides, carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/26Compounds containing silicon or boron, e.g. silica, sand
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/04Elements
    • C10M2201/041Carbon; Graphite; Carbon black
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/105Silica
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/06Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/40Low content or no content compositions
    • C10N2030/42Phosphor free or low phosphor content compositions
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10NINDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2030/00Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
    • C10N2030/40Low content or no content compositions
    • C10N2030/43Sulfur free or low sulfur content compositions

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)

Abstract

The present invention relates to lubrication oil antiwear to damage technical field, and in particular to a kind of preparation method of lubricating oil composite Nano antiwear additive, including:(1) preparation of hydrotalcite precursor;(2) silicon source is reacted to precipitation with fatty amine in water and be wholly absent, then add water-soluble silicate, molybdate, organic titanate, after being well mixed, obtain mixed system 1;(3) hydrotalcite precursor and graphene are added into mixed system 1,3~8h is reacted at 60~120 DEG C, regulation system pH is 3~5, obtains pre-product;(4) after pre-product is calcined in inert gas, lubricating oil composite Nano antiwear additive is obtained;The present invention in hydrotalcite precursor and graphene by adding nano-particle, wear-resisting nano-particle is set to enter between the houghite interlayer and graphene layer of stratiform, abrasion-proof particle is set to be uniformly dispersed in system, and incorporate well in lubricating oil, effectively increase the wear-resistant anti-extreme pressure energy of lubricating oil.

Description

A kind of preparation method of lubricating oil composite Nano antiwear additive
Technical field
The present invention relates to lubrication oil antiwear to damage technical field, and in particular to a kind of lubricating oil composite Nano antiwear additive Preparation method.
Background technology
The main component of lubricating oil includes the lubricating oil addition of lubricating base oil and a variety of organic or inorganics, liquid or solid-state This two large divisions of agent, corresponding lubricating oil is made according to certain ratio compounding in they.Lubricating base oil is broadly divided into mineral base Plinth oil, synthetic base oil and plant oil base oil three major types.With the development of technology, increasing part of appliance will be more Worked under harsh operating mode, thus synthetic lubricant fluid due to its thermal oxidation stability it is good, heat decomposition temperature is high, and resistance to low temperature is good The advantages that, it has also become the base oil component for the lubricating oil that must be used under many special operation conditions.
One of lubricating oil major function is wear-resistant effect, therefore antiwear additive is most important composition portion in lubricating oil / mono-, the function of being directly connected to friction means is realized and efficiency stabilization.Extreme pressure anti-wear additives are that a kind of important lubricating grease adds Add agent, its major part is the compound of some sulfur-bearings, phosphorus, chlorine, lead, molybdenum.In general, chlorine class, sulphur class can improve lubrication The load resistance ability of fat, prevent metal surface from issuing raw burn knot, seizing, scratch in high-load condition;And Phosphorus, organic metal salt Class has higher abrasion-resistance, can prevent or reduce abrasion of the metal surface under the conditions of moderate duty.In practical application, lead to It is more preferable that different types of extreme pressure anti-wear additives are often used in mixed way performance by a certain percentage.
With the continuous development of antiwear additive, the metal nano containing nano metal chemical composition a kind of in the last few years Antiwear additive generates, and this antiwear additive not only has good performance in terms of wear resistence, while also overcomes to ring The influence in border, but it has two aspect deficiencies:First, nano-solution belongs to suspension technology, still it is a kind of unstable after being configured to liquid Fixed liquid, place layering effect occurs for a long time, while add its dispersiveness in lubricating oil and remain larger defect, therefore should Technology needs further to be improved;Second, Nano metal powder, nano-ceramic powder, in parts, engine movements parts surface, make for a long time With that can produce nanoparticle aggregate, this nanometer building-up effect is carried out for a long time, and nano particle is cumulative, is deposited into bulky grain, New abrasion, scuffing of cylinder bore can be produced to parts.Therefore, seek that a kind of wear resistence is excellent, the good lubrication oil antiwear agent of stability turns into industry Boundary's urgent problem to be solved.
The content of the invention
For bad dispersibility of the lubricating oil in the prior art with composite Nano antiwear additive in lubricating oil, friction resistant effect The undesirable deficiency of fruit, it is an object of the invention to provide a kind of lubricating oil composite Nano antiwear additive, and it can be uniform It is dispersed in lubricating oil, and there is excellent friction resistant effect.
To achieve these goals, the present invention is achieved using following technical scheme:
A kind of lubricating oil preparation method of composite Nano antiwear additive, comprises the following steps:
(1) preparation of hydrotalcite precursor:Preparation interlayer anion is NO3-, laminate divalence, Tricationic M2+/M3+'s Hydrotalcite precursor;
(2) silicon source is reacted to precipitation with fatty amine in water and be wholly absent, then add water-soluble silicate, molybdic acid Salt, organic titanate, after being well mixed, obtain mixed system 1;
(3) hydrotalcite precursor and graphene are added into mixed system 1,3~8h, Ran Houjia are reacted at 60~120 DEG C It is 3~5 to enter acidic materials regulation system pH, obtains pre-product;
(4) after pre-product is calcined in inert gas, lubricating oil composite Nano antiwear additive is obtained;
Wherein, M is metal, wherein M2+Selected from Mg2+、Zn2+、Cu2+、Ni2+And Co2+At least one of, M3+Selected from Al3+、 Fe3+And Cr3+At least one of.
The lubricating oil that the present invention is prepared composite Nano antiwear additive, include the graphene of load houghite, And the houghite for nano-particle intercalation nano-particle intercalation houghite wherein, the nano-particle includes nanometer Aluminum oxide, nano silicon, nanoscale molybdenum oxide, nano titanium oxide.Wherein, houghite can be rolled into a ball according to zwitterion Change adjustment interlamellar spacing, have quantity can modulation, the grain size of intercalation assembly and the regulatable feature of distribution, by water Nano-particle is added in talcum precursor, wear-resisting nano-particle is entered between the houghite interlayer and graphene layer of stratiform, makes Abrasion-proof particle can be uniformly dispersed in system, and is incorporated well in lubricating oil, effectively increase the wear-resistant anti-of lubricating oil Extreme pressure property.
By the way that houghite is compound with graphene, it is possible to increase dispersed homogeneous degree of the houghite in lubricating oil, carry The crocking resistance of high lubricating oil;
By nano aluminium oxide, nano silicon, nanoscale molybdenum oxide, nano titanium oxide compound action, by more The interparticle interaction of kind, the anti-wear performance of lubricating oil is further improved, in order to further improve the scattered equal of nano-particle Even property, improves the intercalation efficiency of nano-particle, and under optimum condition, the average grain diameter of the nano aluminium oxide is 50~200 nanometers; The average grain diameter of the nano silicon is 100~300 nanometers;The average grain diameter of the nanoscale molybdenum oxide is received for 50~200 Rice;The average grain diameter of the nano titanium oxide is 100~300 nanometers.
According to the present invention, the preparation method of the hydrotalcite precursor is:By M2+With M3+It is well mixed in aqueous, so After add alkaline matter, regulation pH value of solution is 10~11, in 60~120 DEG C of 4~10h of crystallization, by product centrifuge washing to neutrality, Obtain hydrotalcite precursor.
According to the present invention, as preferable, source of aluminium, water-soluble silicate, molybdate, the weight ratio of organic titanate For 1: (0.1~0.5): (0.05~0.2): (0.5~1).
According to the present invention, the fatty amine is selected from ethylamine, n-butylamine, n-hexyl amine, dodecyl amine, divinyl At least one of triamine, triethylene tetramine.
According to the present invention, in step (4), the time of the calcining is 2~5h, and the temperature of the calcining is 350~600 ℃。
Under the conditions of, according to the invention it is preferred to, on the basis of the parts by weight of source of aluminium 100, the lubricating oil composite Nano Antiwear additive is made up of the material of following parts by weight:M(NO3)2150~250 parts by weight, M (NO3)330~150 parts by weight, alkali Property material 100~120 parts by weight, the parts by weight of silicon source 100, the parts by weight of fatty amine 30~50, the weight of water-soluble silicate 10~50 Part, the parts by weight of molybdate 5~20, the parts by weight of organic titanate 50~100, the parts by weight of acidic materials 50~80, graphene 5~20 Parts by weight, the parts by weight of water 300~500;
Wherein, wherein M (NO3)2Selected from Mg (NO3)2、Zn(NO3)2、Cu(NO3)2、Ni(NO3)2With Co (NO3)2In at least One kind, M (NO3)3Selected from Al (NO3)3、Fe(NO3)3With Cr (NO3)3At least one of.
Under the conditions of, according to the invention it is preferred to, on the basis of the parts by weight of source of aluminium 100, the lubricating oil composite Nano Antiwear additive is made up of the material of following parts by weight:M(NO3)2180~210 parts by weight, M (NO3)345~120 parts by weight, alkali Property material 100~120 parts by weight, the parts by weight of silicon source 100, the parts by weight of fatty amine 30~50, the weight of water-soluble silicate 25~35 Part, the parts by weight of molybdate 8~12, the parts by weight of organic titanate 60~85, the parts by weight of acidic materials 60~78, graphene 10~15 Parts by weight, the parts by weight of water 300~500.
In the present invention, alkaline matter primarily serves regulation pH value of solution, prepares the effect of meta-aluminic acid root, and the present invention does not have to it Special requirement, can be that, for example, in step (2), the alkaline matter is inorganic base well known to one of ordinary skill in the art And/or organic base, it is specifically as follows in alkali metal hydroxide, alkaline earth metal hydroxide, urea and its derivative and organic amine At least one, it is further preferred that the alkaline matter is sodium hydroxide, lithium hydroxide, at least one of potassium hydroxide.
In the present invention, acidic materials mainly play a part of to adjust pH, and it is special that the present invention does not have to the species of acidic materials It is required that can often know for one of ordinary skill in the art, such as the acid source can be inorganic acid and/or organic acid, the nothing Machine acid can be in hydrochloric acid, nitric acid, sulfuric acid, boric acid, perchloric acid, thiocyanic acid, sulfurous acid, phosphoric acid, phosphorous acid, hypochlorous acid etc. extremely Few one kind;The organic acid can be at least one of formic acid, acetic acid, benzoic acid, benzene sulfonic acid etc..
According to the present invention, the species in the present invention for silicon source does not have special requirement, can be art technology people Member often knows, for example, source of aluminium can be aluminium chloride, aluminum sulfate, aluminum nitrate, alumina silicate, aluminium sulfide, alum, aluminium ethide, fourth At least one of base aluminium, aluminium acetate, aluminium triformate, oxalic acid aluminium, propionic acid aluminium etc..
Under the conditions of, according to the invention it is preferred to, the water-soluble silicate is selected from sodium metasilicate and/or potassium silicate.
Under the conditions of, according to the invention it is preferred to, the molybdate is selected from ammonium molybdate or sodium molybdate.
Under the conditions of, according to the invention it is preferred to, the organic titanate is selected from butyl titanate, positive third fat of metatitanic acid, metatitanic acid isopropyl One kind in ester, tetraethyl titanate.
According to the present invention it is possible to the number of functional groups for increasing graphenic surface improves the compound of graphene and houghite Spend, under optimum condition, the graphene is redox graphene.
The lubricating oil composite Nano antiwear additive that the present invention obtains can be adjusted directly with commercially available lubricating oil ultrasound ball milling With into required wearproof lubricant, the processing without carrying out step complexity to all base oils or lubricating oil, so as to save Save the cost for preparing extreme-pressure wear-resistant lubricating oil and reduced and prepare extreme-pressure wear-resistant Lubricating Oil Technique difficulty.
Compared with prior art, the present invention has following technique effect:
The present invention makes wear-resisting nano-particle enter stratiform by adding nano-particle in hydrotalcite precursor and graphene Houghite interlayer and graphene layer between, abrasion-proof particle is uniformly dispersed in system, and well incorporate lubrication In oil, the wear-resistant anti-extreme pressure energy of lubricating oil is effectively increased, and the change that houghite can be rolled into a ball according to zwitterion adjusts Interlamellar spacing, have quantity can modulation, the grain size of intercalation assembly and the regulatable feature of distribution, friction can be reduced, drop Low component wear, improve power output and reduce fuel oil loss, and the not corrosive substance such as sulfur-bearing, phosphorus, do not have in itself to parts Infringement, not generation environment pollution.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below Specific embodiment is closed, the present invention is furture elucidated.
Embodiment 1
A kind of preparation method of lubricating oil composite Nano antiwear additive:
(1) by 200g Mg (NO3)2With 80g Al (NO3)3It is well mixed in aqueous, then adds 110g hydroxides Sodium, regulation pH value of solution is 10.5, in 100 DEG C of crystallization 6h, by product centrifuge washing to neutrality, obtains hydrotalcite precursor;
(2) 100g aluminium chloride is reacted to precipitation with 40g ethylamines in water and is wholly absent, then add 30g sodium metasilicate, 10g ammonium molybdates, 7g butyl titanates, after being well mixed, obtain mixed system 1;
(3) hydrotalcite precursor and 12g graphenes are added into mixed system 1,5h is reacted at 90 DEG C, then adds 70g Hydrochloric acid regulation system pH is 4, obtains pre-product;
(4) by pre-product in nitrogen with 450 DEG C of temperature calcination 3h after, obtain the wear-resistant addition of lubricating oil composite Nano Agent;
The lubricating oil that the present embodiment is prepared composite Nano antiwear additive, include the graphite of load houghite Alkene, the houghite are the houghite of nano-particle intercalation;
Wherein, the nano-particle is nano aluminium oxide, nano silicon, nanoscale molybdenum oxide and nano titanium oxide Mixture;
The weight ratio of the graphene and the houghite is 1:0.15.
Embodiment 2
A kind of preparation method of lubricating oil composite Nano antiwear additive:
(1) by 180g Zn (NO3)2With 45g Al (NO3)3It is well mixed in aqueous, then adds 100g hydroxides Potassium, regulation pH value of solution is 10.5, in 80 DEG C of crystallization 5h, by product centrifuge washing to neutrality, obtains hydrotalcite precursor;
(2) 100g aluminum sulfate is reacted to precipitation with 30g n-butylamines in water and be wholly absent, then add 25g silicic acid Sodium, 8g ammonium molybdates, 60g tetraethyl titanates, after being well mixed, obtain mixed system 1;
(3) hydrotalcite precursor and 10g graphenes are added into mixed system 1,4h is reacted at 70 DEG C, then adds 60g Nitric acid regulation system pH is 4, obtains pre-product;
(4) by pre-product in nitrogen with 400 DEG C of temperature calcination 4h after, obtain the wear-resistant addition of lubricating oil composite Nano Agent;
The lubricating oil that the present embodiment is prepared composite Nano antiwear additive, include the graphite of load houghite Alkene, the houghite are the houghite of nano-particle intercalation;
Wherein, the nano-particle is nano aluminium oxide, nano silicon, nanoscale molybdenum oxide and nano titanium oxide Mixture;
The weight ratio of the graphene and the houghite is 1:0.1.
Embodiment 3
A kind of preparation method of lubricating oil composite Nano antiwear additive:
(1) by 210g Cu (NO3)2With 120g Fe (NO3)3It is well mixed in aqueous, then adds 120g hydroxides Sodium, regulation pH value of solution is 10.8, in 110 DEG C of crystallization 9h, by product centrifuge washing to neutrality, obtains hydrotalcite precursor;
(2) 100g aluminum nitrates are reacted to precipitation with 50g n-hexyl amine in water and be wholly absent, then add 35g silicic acid Sodium, 12g ammonium molybdates, 85g butyl titanates, after being well mixed, obtain mixed system 1;
(3) hydrotalcite precursor and 15g graphenes are added into mixed system 1,7h is reacted at 110 DEG C, then adds 78g Sulfuric acid regulation system pH is 5, obtains pre-product;
(4) by pre-product in nitrogen with 500 DEG C of temperature calcination 4h after, obtain the wear-resistant addition of lubricating oil composite Nano Agent;
The lubricating oil that the present embodiment is prepared composite Nano antiwear additive, include the graphite of load houghite Alkene, the houghite are the houghite of nano-particle intercalation;
Wherein, the nano-particle is nano aluminium oxide, nano silicon, nanoscale molybdenum oxide and nano titanium oxide Mixture;
The weight ratio of the graphene and the houghite is 1:0.25.
Embodiment 4
A kind of preparation method of lubricating oil composite Nano antiwear additive:
(1) by 150g Ni (NO3)2With 30g Fe (NO3)3It is well mixed in aqueous, then adds 100g hydroxides Potassium, regulation pH value of solution is 10, in 60 DEG C of crystallization 10h, by product centrifuge washing to neutrality, obtains hydrotalcite precursor;
(2) 100g alumina silicate is reacted to precipitation with 30g dodecyl amine in water and be wholly absent, then add 10g Positive third fat of sodium metasilicate, 5g sodium molybdates, 50g metatitanic acids, after being well mixed, obtain mixed system 1;
(3) hydrotalcite precursor and 5g graphenes are added into mixed system 1,8h is reacted at 60 DEG C, then adds boric acid Regulation system pH is 3, obtains pre-product;
(4) by pre-product in nitrogen with 600 DEG C of temperature calcination 2h after, obtain the wear-resistant addition of lubricating oil composite Nano Agent;
The lubricating oil that the present embodiment is prepared composite Nano antiwear additive, include the graphite of load houghite Alkene, the houghite are the houghite of nano-particle intercalation;
Wherein, the nano-particle is nano aluminium oxide, nano silicon, nanoscale molybdenum oxide and nano titanium oxide Mixture;
The weight ratio of the graphene and the houghite is 1:0.05.
Embodiment 5
A kind of preparation method of lubricating oil composite Nano antiwear additive:
(1) by 250g Cu (NO3)2With 150g Cr (NO3)3It is well mixed in aqueous, then adds 120g hydroxides Sodium, regulation pH value of solution is 11, in 120 DEG C of crystallization 4h, by product centrifuge washing to neutrality, obtains hydrotalcite precursor;
(2) 100g aluminium chloride is reacted to precipitation with 50g ethylamines in water and is wholly absent, then add 50g potassium silicates, 20g sodium molybdates, 100g isopropyl titanates, after being well mixed, obtain mixed system 1;
(3) hydrotalcite precursor and 20g graphenes are added into mixed system 1,3h is reacted at 120 DEG C, then adds 80g Phosphoric acid regulation system pH is 5, obtains pre-product;
(4) by pre-product in nitrogen with 350 DEG C of temperature calcination 5h after, obtain the wear-resistant addition of lubricating oil composite Nano Agent;
The lubricating oil that the present embodiment is prepared composite Nano antiwear additive, include the graphite of load houghite Alkene, the houghite are the houghite of nano-particle intercalation;
Wherein, the nano-particle is nano aluminium oxide, nano silicon, nanoscale molybdenum oxide and nano titanium oxide Mixture;
The weight ratio of the graphene and the houghite is 1:0.3.
Comparative example 1
The dosage of sodium metasilicate in embodiment 1 is adjusted to 5g, remaining is constant, and described lubricating oil is prepared and is received with compound Rice antiwear additive.
Comparative example 2
The dosage of sodium metasilicate in embodiment 1 is adjusted to 60g, remaining is constant, and described lubricating oil is prepared with compound Nano abrasion-resistant additive.
Comparative example 3
The dosage of ammonium molybdate in embodiment 1 is adjusted to 2g, remaining is constant, and described lubricating oil is prepared and is received with compound Rice antiwear additive.
Comparative example 4
The dosage of ammonium molybdate in embodiment 1 is adjusted to 30g, remaining is constant, and described lubricating oil is prepared with compound Nano abrasion-resistant additive.
It is specific as follows there is provided endurance check in order to contrast effect of the present invention:
This test method uses four-ball test method, and four-ball test parameter and standard is:Rotating speed 1500r/min, load 400N, Time 2h.This experiment steel ball used manufactures according to GB/308-89, GCr15, two level steel ball, diameter 13.4mm, hardness 64- 66HRC。
Test oil is that 20# standard mechanicals oil does not add the lubricating oil of above-described embodiment 1~5 and comparative example 1~4 with again Nano abrasion-resistant additive is closed, in experiment, test oil is injected in the lubricating cup for accommodating steel ball, liquid level was not had the table of steel ball just Face, it is 400N to apply vertical load P, moment of friction is measured, by formula:(wherein μ is friction factor for μ=0.233 × T/P;T For moment of friction) friction factor is calculated, once it is used for the friction factor μ and wear extent for evaluating detection oil.Experiment is front and rear to steel Ball and ring block are fully cleaned, and the wear extent of steel ball, is shown with metallographic before and after then being tested with a ten thousandth electronic balance weighing Micro mirror measures the wear scar diameter of steel ball, and correction data is as follows:
Quality (g) before mill Quality (g) after mill Mass Loss (g)
Embodiment 1 36.4177 36.4173 0.0004
Embodiment 2 36.4057 36.405 0.0007
Embodiment 3 36.4136 36.4128 0.0008
Embodiment 4 36.3874 36.3866 0.0008
Embodiment 5 36.4016 36.4008 0.0008
Comparative example 1 36.4127 36.4108 0.0019
Comparative example 2 36.3874 36.3851 0.0023
Comparative example 3 36.4159 36.4134 0.0025
Comparative example 4 36.4126 36.4091 0.0035
The steel ball surface corresponding to comparative example it can be seen from data above 1~4 has an obvious wear phenomenon, and this hair The steel ball surface wear extent of embodiment 1~5 is minimum corresponding to bright.
General principle, principal character and the features of the present invention of the present invention has been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes Change and improvement is both fallen within the range of claimed invention.The scope of protection of present invention is by appended claims And its equivalent thereof.

Claims (5)

  1. A kind of 1. lubricating oil preparation method of composite Nano antiwear additive, it is characterised in that:Comprise the following steps:
    (1) preparation of hydrotalcite precursor:Preparation interlayer anion is NO3-, laminate divalence, Tricationic M2+/M3+Neatly Stone precursor;
    (2) silicon source is reacted to precipitation with fatty amine in water and be wholly absent, then added water-soluble silicate, molybdate, have Organic titanate, after being well mixed, obtain mixed system 1;
    (3) hydrotalcite precursor and graphene are added into mixed system 1,3~8h is reacted at 60~120 DEG C, then adds acid Property material regulation system pH be 3~5, obtain pre-product;
    (4) after pre-product is calcined in inert gas, lubricating oil composite Nano antiwear additive is obtained;
    Wherein, M is metal, wherein M2+Selected from Mg2+、Zn2+、Cu2+、Ni2+And Co2+At least one of, M3+Selected from Al3+、Fe3+ And Cr3+At least one of.
  2. 2. the lubricating oil according to claim 1 preparation method of composite Nano antiwear additive, it is characterised in that:It is described Silicon source, water-soluble silicate, molybdate, the weight ratio of organic titanate are 1:(0.1~0.5):(0.05~0.2):(0.5~ 1)。
  3. 3. the lubricating oil according to claim 1 preparation method of composite Nano antiwear additive, it is characterised in that:It is described Fatty amine is selected from ethylamine, n-butylamine, n-hexyl amine, dodecyl amine, diethylenetriamine, in triethylene tetramine at least It is a kind of.
  4. 4. the lubricating oil according to claim 1 preparation method of composite Nano antiwear additive, it is characterised in that:It is described The time of calcining is 2~5h, and the temperature of the calcining is 350~600 DEG C.
  5. 5. the lubricating oil according to claim 1 preparation method of composite Nano antiwear additive, it is characterised in that:It is described The preparation method of hydrotalcite precursor is:By M2+With M3+It is well mixed in aqueous, then adds alkaline matter, adjusts solution PH is 10~11, in 60~120 DEG C of 4~10h of crystallization, by product centrifuge washing to neutrality, obtains hydrotalcite precursor.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108441288A (en) * 2018-05-02 2018-08-24 合肥博创机械制造有限公司 A kind of novel lubricating oil additive and preparation method thereof
CN109722323A (en) * 2019-01-04 2019-05-07 清华大学 A kind of preparation method of polyethers hydrotalcite mixed solution
CN110305712A (en) * 2019-07-16 2019-10-08 成都新柯力化工科技有限公司 A kind of lube oil additive and preparation method of phyllosilicate loaded graphene

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5578286A (en) * 1994-04-29 1996-11-26 Aluminum Company Of America Two powder synthesis of hydrotalcite-like compounds with divalent or polyvalent organic anions
CN104071756B (en) * 2014-06-24 2015-12-02 太原理工大学 A kind of MnO 2the preparation method of intercalation hydrotalcite-like composite material
CN104893786B (en) * 2015-05-28 2017-06-30 清华大学 A kind of preparation and application method of hydrotalcite nano additive
CN107523375B (en) * 2017-08-22 2020-01-31 辽宁汽众润滑油生产有限公司 antiwear agent special for lubricating oil and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108441288A (en) * 2018-05-02 2018-08-24 合肥博创机械制造有限公司 A kind of novel lubricating oil additive and preparation method thereof
CN109722323A (en) * 2019-01-04 2019-05-07 清华大学 A kind of preparation method of polyethers hydrotalcite mixed solution
CN110305712A (en) * 2019-07-16 2019-10-08 成都新柯力化工科技有限公司 A kind of lube oil additive and preparation method of phyllosilicate loaded graphene
CN110305712B (en) * 2019-07-16 2021-11-12 哈尔滨华帆科技发展有限公司 Layered silicate loaded graphene lubricating oil additive and preparation method thereof

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