CN100334187C - Method for preparing nano lubricating fluid comprising oleophilic metal sulfide - Google Patents

Method for preparing nano lubricating fluid comprising oleophilic metal sulfide Download PDF

Info

Publication number
CN100334187C
CN100334187C CNB2005101302584A CN200510130258A CN100334187C CN 100334187 C CN100334187 C CN 100334187C CN B2005101302584 A CNB2005101302584 A CN B2005101302584A CN 200510130258 A CN200510130258 A CN 200510130258A CN 100334187 C CN100334187 C CN 100334187C
Authority
CN
China
Prior art keywords
nano
lubricating oil
reaction
preparation
lubricating fluid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CNB2005101302584A
Other languages
Chinese (zh)
Other versions
CN1775933A (en
Inventor
朱红
王滨
郭洪范
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beijing Jiaotong University
Original Assignee
Beijing Jiaotong University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beijing Jiaotong University filed Critical Beijing Jiaotong University
Priority to CNB2005101302584A priority Critical patent/CN100334187C/en
Publication of CN1775933A publication Critical patent/CN1775933A/en
Application granted granted Critical
Publication of CN100334187C publication Critical patent/CN100334187C/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Lubricants (AREA)

Abstract

The present invention relates to a method for preparing metallic sulfide nano lubricating fluid with lipophilicity. The present invention takes organic metallic salt precursors and hydrogen sulfide gas as reactants to directly synthesize the mother solution of metallic sulfide nano-particles with lipophilicity from lubricating oil by way of in-situ synthesis, and metallic sulfide nano lubricating fluid with lipophilicity is obtained after the mother solution is directly conditioned and agitated together with the lubricating oil. The synthetic nano lubricating fluid of the present invention has good dispersion stability, the generation of nano-particles in the process of synthesis and surface modification are synchronously completed, and only nano-particles and surface modifiers but not surplus byproducts are generated in reaction. The present invention well solves the problem that nano-materials have poor dispersion stability in lubricating oil, and has the advantages of simple operation, no need of special technical equipment and easy industrialization. The nano lubricating fluid prepared in the present invention can reduce the friction coefficient, shorten the friction spot diameter and achieve the effects of wear resistance and friction reduction.

Description

A kind of preparation method of nano lubricating fluid comprising oleophilic metal sulfide
Technical field
The present invention relates to a kind of preparation method who contains the lubricating fluid of nano material.
Background technology
The developmental level of lubricating oil additive is to weigh the important symbol of a national quality of lubrication oil.In recent years, because inorganic nano material has the special physicochemical performance, the research that nano material is applied to lubricating oil additive has been subjected to increasing attention.But because the surface of most of inorganic nano materials has hydrophobicity, it is dispersed in the lubricant medium through leaving standstill for a long time has deposited phenomenon and take place, this has limited inorganic nano material greatly in the lubricating oil additive Application for Field.And the interpolation of nano material to be having good dispersion and the long-acting prerequisite that stabilizes in lubricant medium, otherwise not only is difficult to bring into play its excellent tribological property, and in use stops up oil circuit and purifier because of reunion.Therefore, resolving the dispersion stabilization problem of nano material in the lubricating oil medium is one of gordian technique that nano material is applied to the lubricating oil additive field.
Inorganic nano material also is in the starting stage as the research of lubricating oil additive at present, and many basic research work also need to carry out energetically, especially solves the dispersion stabilization problem of inorganic nano material in lubricated wet goods organic medium.In order to improve its dispersion stabilization in lubricating oil, need carry out surface modification to inorganic nano material, thereby it can be used as lubricating oil additive.Preparation at present mainly contains two kinds as the method for the nano material of lubricating oil additive: first method is to prepare nano material earlier, with dispersion agent nano material is suspended in the lubricant medium again and uses as lubricating oil additive, as Chinese patent CN 1175621A, CN 1536058A.The deficiency of this method is that the finishing of nano material is complete inadequately, and nano material is distributed to often needs in the lubricating oil medium by technologies such as ultrasonic, violent mechanical stirring, for having relatively high expectations and shortcoming such as complex manufacturing technology of equipment; Second method is to add the chemical surface modifier in water or pure water mixed phase isopolarity reaction system, synthesize by chemical reaction and to have oil loving nano material, again it is scattered in nano material in the lubricated wet goods medium by certain dispersing method, as Chinese patent CN 1183461A, CN 1221748A, CN 1354056A.The deficiency of this method is owing to be the nano material of preparing in polar solvent, the surface hydrophilicity of nano material can strengthen to some extent, lipophilicity is not fine, and the post-processed work of nano material preparation as processes such as filtration, dryings in, the caking of nano material takes place easily.This shows, though these two kinds of methods have solved the compatibility issue between inorganic nano material and the lubricated wet goods nonpolar medium to a certain extent, but can only obtain the stably dispersing of short-term, through leaving standstill for a long time the change of inorganic nano material particle diameter still can appear greatly, phenomenons such as reunion take place, thereby had a strong impact on the quality of lubricating oil, and nano material has been dispersed in the lubricated wet goods lubricant medium complex manufacturing technology, the more high shortcoming of equipment requirements are arranged.
Summary of the invention
It is poor to the objective of the invention is at nano material dispersion stabilization in lubricated wet goods nonpolar medium, nano material is problem such as dispersing technology complexity in lubricated wet goods medium, a kind of directly method of original position nano materials in lubricated wet goods nonpolar medium is provided, directly the mother liquor that contains the higher concentration nano particle that is synthesized and lubricating oil are in harmonious proportion stirring then, promptly obtain containing the lubricating fluid of nano particle.
Technical scheme of the present invention:
A) preparation of organic metal salt presoma
Step 1 joins the mixed solvent of normal hexane and dehydrated alcohol in the reaction vessel, and then to add reaction raw materials 1 concentration range be the copper chloride solution of 0.5~2mol/L, and wherein three's volume ratio is 7: 4: 3;
Step 2 joins reaction raw materials 2 sodium oleates in the above-mentioned reaction vessel, and wherein the mol ratio of cupric chloride and sodium oleate is 1: 2, reacts 2~5h under 65~85 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 50~60 ℃ of conditions to organic phase, removes organic solvent and obtains the organic metal salt presoma;
B) original position of oleophilic metal sulfide is synthetic
Step 1 joins above-mentioned organic metal salt presoma and coating materials oleic acid in another reaction vessel, and both mol ratios are 1: 2~2: 1;
Step 2 adds lubricating oil as reaction medium again in reaction vessel, wherein the content of organic metal salt presoma in lubricating oil is 0.1~1mol/Kg;
Step 3, the material in the reacting by heating container also keeps 25~35 ℃, is stirred to the organic metal salt presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, under 25~45 ℃ of temperature of reaction, continue stirring reaction 2~4h, and promptly obtaining concentration is w 1The mother liquor that contains the oleophilic metal sulfide nano particle, w 1Scope be 1.00~10.0%;
Concentration w 1 = M × n W × 100 %
Wherein M is the formula weight of metallic sulfide; N is the amount of substance of metallic sulfide, unit: mol; W is the quality of lubricating oil, unit: g;
C) preparation of nano lubricating fluid
With quality is m 1Above-mentioned mother liquor and quality be m 2Lubricating oil be in harmonious proportion stirring, promptly obtaining concentration is w 2Nano lubricating fluid, w 2Scope be 0.05~3.00%, determine the add-on m of lubricating oil according to following formula 2
m 2 = ( w 1 - w 2 ) × m 1 w 2
The described mixed solvent of step 1 can also use the mixed solvent of normal heptane and dehydrated alcohol in the preparation of organic metal salt presoma, and its volume ratio is 7: 4.
The described reaction raw materials 1 of step 1 can also use the aqueous solution of copper sulfate, cupric nitrate, neutralized verdigris, nickelous chloride, single nickel salt, zinc chloride, zinc sulfate, zinc nitrate, zinc acetate, lead chloride, lead nitrate or plumbic acetate in the preparation of organic metal salt presoma, and its concentration range is 0.5~2mol/L.
The described reaction raw materials 2 of step 2 can also use potassium oleate in the preparation of organic metal salt presoma.
The described lubricating oil of step 2 is meant cut lubricating oil, hydro carbons lubricating oil, polyether class lubricating oil or silicone oil lubricating oil in the original position of oleophilic metal sulfide is synthetic.
In the preparation of organic metal salt presoma, the described mixed solvent of step 1 selects for use normal hexane and dehydrated alcohol for best, the described reaction raw materials 1 of step 1 selects for use cupric chloride, nickelous chloride for best, it is best that the described reaction raw materials 2 of step 2 is selected sodium oleate for use, and the optimum temps of the heating described in the step 2 is 70 ℃.In the original position building-up process of oleophilic metal sulfide, described organic metal salt presoma of step 1 and the oleic optimum mole ratio of coating materials are 1: 1.The described temperature of reaction of step 3, from saving the angle of the energy, the original position that can consider directly at room temperature to carry out oleophilic metal sulfide is synthetic.
The beneficial effect that the present invention has:
1. the oil loving nano metal sulfide particle grain of the present invention preparation, because surface modification is directly to carry out in the lubricating oil medium, so nano particle not only has good lipophilicity, and has better dispersion stabilization in lubricating oil.
2. this directly method of original position ucon oil additive in the lubricating oil medium of the present invention's proposition has only the generation of nano particle and coating materials in the building-up process, does not have unnecessary by product to generate, and has the simple advantage of operating process.
The present invention propose this directly in the lubricating oil medium method of original position ucon oil additive need not through traditional step as drying, filtration, washing etc., also need not nano particle joined it by means such as ultrasonic, vigorous stirring and lubricate in the wet goods medium.Only need mother liquor and lubricating oil mediation stirring can be obtained nano lubricating fluid.Therefore this invention has the characteristics not high to equipment requirements.
Description of drawings
Fig. 1 original position synthetic oleic acid modified nano copper sulfate particle transmission shape appearance figure.
Fig. 2 original position synthetic oleic acid modified nanometer nickel sulfide particle transmission shape appearance figure.
Fig. 3 copper sulphide nano lubricating oil additive adds the change curve of The friction coefficient interpolation concentration under the concentration in difference.
Fig. 4 nanometer nickel sulfide lubricating oil additive adds the change curve of The friction coefficient interpolation concentration under the concentration in difference.
Fig. 5 copper sulphide nano lubricating oil additive adds under the concentration wear scar diameter with the change curve that adds concentration in difference.
Fig. 6 nanometer nickel sulfide lubricating oil additive adds under the concentration wear scar diameter with the change curve that adds concentration in difference.
Wear scar diameter sem photograph under Fig. 7 straight lubrication oil lubricating condition (magnification * 100, * 1000).
Fig. 8 contains wear scar diameter sem photograph (magnification * 100, * 1000) under the 0.1% lipophilicity nano copper sulfate particle condition.
Fig. 9 contains wear scar diameter sem photograph (magnification * 100, * 1000) under the 0.3% lipophilicity nanometer nickel sulfide particle condition.
Embodiment
By example the specific embodiment of the present invention is described.
Example 1
A) preparation of organo-metallic mantoquita presoma
Step 1 joins the mixed solvent of 70mL normal hexane and 40mL dehydrated alcohol in the reaction vessel, and then to add reaction raw materials concentration be 0.667mol/L copper chloride solution 30mL;
Step 2 joins 0.04mol reaction raw materials sodium oleate in the above-mentioned reaction vessel, reacts 3h under 70 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 60 ℃ of conditions to organic phase, removes organic solvent and obtains organo-metallic mantoquita presoma;
B) original position of oleophilic metal cupric sulfide is synthetic
Step 1 joins 0.02mol organo-metallic mantoquita presoma and 0.02mol oleic acid in another reaction vessel;
Step 2 adds 100g hydro carbons lubricating oil as reaction medium again in reaction vessel, wherein the content of organo-metallic mantoquita presoma in lubricating oil is 0.2mol/Kg;
Step 3, the material in the reacting by heating container also keeps 30 ℃, is stirred to organo-metallic mantoquita presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, at 25 ℃ of following stirring reaction 4h, promptly obtain concentration and be 1.92% the mother liquor that contains the lipophilicity nano copper sulfate particle;
The calculation formula of concentration is: w 1 = M × n W × 100 % ,
Wherein M is the formula weight of metallic sulfide; N is the amount of substance of metallic sulfide, unit: mol; W is the quality of lubricating oil, unit: g;
C) preparation of nano lubricating fluid
The above-mentioned mother liquor of getting 2.0g, 4.0g, 8.0g, 10.0g, 20.0g successively is in harmonious proportion stirring with 74.8g, 72.8g, 43.2g, 28.4g, 18.4g hydro carbons lubricating oil respectively, promptly obtaining concentration is 0.05%, 0.1%, 0.3%, 0.5%, 1.0% contains lipophilicity copper sulphide nano lubricating fluid.
Determine the add-on m of lubricating oil according to following formula 2
m 2 = ( w 1 - w 2 ) × m 1 w 2 M wherein 1Be the quality of mother liquor, w 1Be the concentration of mother liquor, m 2Be the add-on of lubricating oil, w 2Concentration for nano lubricating fluid.
This example approach is an optimum implementation.
Example 2
A) preparation of organo-metallic mantoquita presoma
Step 1 joins the mixed solvent of 7L normal heptane and 4L dehydrated alcohol in the reaction vessel, and then to add reaction raw materials concentration be 2mol/L copper sulfate solution 3L;
Step 2 joins 12mol reaction raw materials sodium oleate in the above-mentioned reaction vessel, reacts 5h under 85 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 55 ℃ of conditions to organic phase, removes organic solvent and obtains organo-metallic mantoquita presoma;
B) original position of oleophilic metal cupric sulfide is synthetic
Step 1 joins 2mol organo-metallic mantoquita presoma and 3mol oleic acid in another reaction vessel;
Step 2 adds the 2Kg polyether class lubricating oil as reaction medium again in reaction vessel, wherein the content of organo-metallic mantoquita presoma in lubricating oil is 1mol/Kg;
Step 3, the material in the reacting by heating container also keeps 32 ℃, is stirred to organo-metallic mantoquita presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, at 40 ℃ of following stirring reaction 2.5h, promptly obtain concentration and be 9.6% the mother liquor that contains the lipophilicity nano copper sulfate particle;
C) preparation of nano lubricating fluid
The above-mentioned mother liquor of getting 20.0g, 50.0g, 80.0g, 100.0g, 120.0g successively is in harmonious proportion stirring with 364.0g, 430.0g, 432.0g, 380.0g, 264.0g polyether class lubricating oil respectively, promptly obtaining concentration is 0.5%, 1.0%, 1.5%, 2.0%, 3.0% contains lipophilicity copper sulphide nano lubricating fluid.
Example 3
A) preparation of organo-metallic nickel salt presoma
Step 1 joins the mixed solvent of 140mL normal hexane and 80mL dehydrated alcohol in the reaction vessel, and then to add reaction raw materials concentration be 0.667mol/L nickel chloride aqueous solution 60mL;
Step 2 joins 0.08mol reaction raw materials sodium oleate in the above-mentioned reaction vessel, reacts 2.5h under 68 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 62 ℃ of conditions to organic phase, removes organic solvent and obtains organo-metallic nickel salt presoma;
B) original position of oleophilic metal nickelous sulfide is synthetic
Step 1 joins 0.04mol organo-metallic nickel salt presoma and 0.04mol oleic acid in another reaction vessel;
Step 2 adds 200g hydro carbons lubricating oil as reaction medium again in reaction vessel, wherein the content of organo-metallic nickel salt presoma in lubricating oil is 0.2mol/Kg;
Step 3, the material in the reacting by heating container also keeps 32 ℃, is stirred to organo-metallic nickel salt presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, at 28 ℃ of following stirring reaction 3h, promptly obtain concentration and be 1.81% contain lipophilicity nanometer nickel sulfide particulate mother liquor;
C) preparation of nano lubricating fluid
The above-mentioned mother liquor of getting 2.0g, 4.0g, 8.0g, 10.0g, 20.0g successively is in harmonious proportion stirring with 70.4g, 68.4g, 40.3g, 26.2g, 16.2g hydro carbons lubricating oil respectively, promptly obtaining concentration is 0.05%, 0.1%, 0.3%, 0.5%, 1.0% contains lipophilicity nanometer nickel sulfide lubricating fluid.
Example 4
A) preparation of organo-metallic nickel salt presoma
Step 1 joins the mixed solvent of 3.5L normal heptane and 2L dehydrated alcohol in the reaction vessel, and then to add reaction raw materials concentration be 0.8mol/L nickel sulfate solution 1.5L;
Step 2 joins 2.4mol reaction raw materials potassium oleate in the above-mentioned reaction vessel, reacts 3.5h under 84 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 50 ℃ of conditions to organic phase, removes organic solvent and obtains organo-metallic nickel salt presoma;
B) original position of oleophilic metal cupric sulfide is synthetic
Step 1 joins 1mol organo-metallic nickel salt presoma and 2mol oleic acid in another reaction vessel;
Step 2 adds 2Kg silicone oil lubricating oil as reaction medium again in reaction vessel, wherein the content of organo-metallic nickel salt presoma in lubricating oil is 0.5mol/Kg;
Step 3, the material in the reacting by heating container also keeps 35 ℃, is stirred to organo-metallic nickel salt presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, at 38 ℃ of following stirring reaction 3h, promptly obtain concentration and be 4.53% contain lipophilicity nanometer nickel sulfide particulate mother liquor;
C) preparation of nano lubricating fluid
The above-mentioned mother liquor of getting 25.0g, 50.0g, 80.0g, 100.0g, 150.0g successively is in harmonious proportion stirring with 201.5g, 252.0g, 282.4g, 202.0g, 189.8g silicone oil lubricating oil respectively, promptly obtaining concentration is 0.5%, 0.75%, 1.0%, 1.5%, 2.0% contains lipophilicity nanometer nickel sulfide lubricating fluid.
Example 5
A) preparation of organo-metallic zinc salt presoma
Step 1 joins the mixed solvent of 700mL normal hexane and 400mL dehydrated alcohol in the reaction vessel, and then to add reaction raw materials concentration be 0.75mol/L solder(ing)acid 300mL;
Step 2 joins 0.45mol reaction raw materials potassium oleate in the above-mentioned reaction vessel, reacts 4.5h under 75 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 58 ℃ of conditions to organic phase, removes organic solvent and obtains organo-metallic nickel salt presoma;
B) original position of oleophilic metal zinc sulphide is synthetic
Step 1 joins 0.2mol organo-metallic zinc salt presoma and 0.1mol oleic acid in another reaction vessel;
Step 2 adds 0.5Kg silicone oil lubricating oil as reaction medium again in reaction vessel, wherein the content of organo-metallic zinc salt presoma in lubricating oil is 0.4mol/Kg;
Step 3, the material in the reacting by heating container also keeps 34 ℃, is stirred to organo-metallic zinc salt presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, at 42 ℃ of following stirring reaction 2h, promptly obtain concentration and be 3.88% the mother liquor that contains the lipophilicity zine sulfide nano particles;
C) preparation of nano lubricating fluid
The above-mentioned mother liquor of getting 20.0g, 50.0g, 80.0g, 100.0g, 120.0g successively is in harmonious proportion stirring with 135.2g, 208.7g, 230.4g, 158.7g, 112.8g cut lubricating oil respectively, promptly obtaining concentration is 0.5%, 0.75%, 1.0%, 1.5%, 2.0% contains lipophilicity zinc sulfide nano lubricating fluid.
Example 6
A) preparation of organo-metallic lead salt presoma
Step 1 joins the mixed solvent of 1.4L normal hexane and 0.8L dehydrated alcohol in the reaction vessel, and then to add reaction raw materials concentration be 0.05mol/L lead acetate water solution 0.6L;
Step 2 joins 0.06mol reaction raw materials potassium oleate in the above-mentioned reaction vessel, reacts 5h under 82 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 57 ℃ of conditions to organic phase, removes organic solvent and obtains organo-metallic nickel salt presoma;
B) original position of oleophilic metal zinc sulphide is synthetic
Step 1 joins 0.03mol organo-metallic lead salt presoma and 0.05mol oleic acid in another reaction vessel;
Step 2 adds 0.3Kg silicone oil lubricating oil as reaction medium again in reaction vessel, wherein the content of organo-metallic zinc salt presoma in lubricating oil is 0.1mol/Kg;
Step 3, the material in the reacting by heating container also keeps 35 ℃, is stirred to organo-metallic zinc salt presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, at 30 ℃ of following stirring reaction 4.5h, promptly obtain concentration and be 2.39% the mother liquor that contains the lipophilicity zine sulfide nano particles;
C) preparation of nano lubricating fluid
The above-mentioned mother liquor of getting 10.0g, 15.0g, 20.0g, 25.0g, 30.0g successively is in harmonious proportion stirring with 18.9g, 56.7g, 43.7g, 34.8g, 5.9g hydro carbons lubricating oil respectively, promptly obtaining concentration is 0.25%, 0.5%, 0.75%, 1.0%, 2.0% contains lipophilicity lead sulfide nano lubricating fluid.
The performance evaluation of nano lubricating fluid:
Fig. 1 is example 1 an original position synthetic oleic acid modified nano copper sulfate particle transmission shape appearance figure.Fig. 2 is example 3 original position synthetic oleic acid modified nanometer nickel sulfide particle transmission shape appearance figures.As can be seen from the figure, no tangible agglomeration between nano particle.This is because the surface of inorganic nanoparticles is coated with one deck organic decoration layer, has reduced the surface energy of nano particle, has reduced the interaction force between nano particle, has stoped its reunion.Nano lubricating fluid is placed the reunion that nano particle can not take place for a long time, and this mainly is that the finishing of nano particle is simultaneously also carried out in lubricating oil because nano particle is directly synthetic in nonpolar lubricating oil.Just because of between coating materials and nano particle chemisorption having taken place, make nano particle have lipophilicity preferably, thereby strengthened the dispersion stabilization of nano particle in lubricating oil.
The nano lubricating fluid comprising oleophilic metal sulfide that example 1 and example 3 obtain is investigated its antiwear and friction reduction property on U.S. home-made FALEX-6 type four-ball tester.Test conditions is that the speed of mainshaft is 1450r/min, and load is 300N, and test period is 30min, and test temperature is a room temperature condition.Special-purpose GCr15 (AISI 52100) the ten grade standard steel balls of four-ball tester that used steel ball is produced for Shanghai Bearing Factory, diameter 12.7mm, hardness 62~64HRC.The concentration of testing used nano lubricating fluid is 0.05%, 0.1%, 0.3%, 0.5%, 1.0%.After the off-test, be the grinding defect diameter that the direct-reading type microscope of 0.01mm is tried under measuring 3 on the horizontal direction of polishing scratch and the vertical direction with precision, ask its mean value as test result, the difference of 3 parallel test results and mean value is not more than 5%; After friction-wear test finishes steel ball is total to 10min 3 times with the sherwood oil ultrasonic cleaning, seasoning adopts JEOL JSM35 type scanning electronic microscope (SEM) that observation analysis has been carried out on mill spot surface.
The oleophilic metal nano copper sulfate particle can significantly reduce the frictional coefficient of lubricating oil and reduce the degree of wear as can be seen from Fig. 3 and Fig. 5, and frictional coefficient and wear scar diameter all are to be the big trend in earlier little back with adding concentration, adding concentration is 0.1% o'clock, and frictional coefficient and wear scar diameter reach minimum value.
Oleophilic metal nanometer nickel sulfide particle also can significantly reduce the frictional coefficient of lubricating oil and reduce the degree of wear as can be seen from Fig. 4 and Fig. 6, and frictional coefficient and wear scar diameter all are to be the big trend in earlier little back with adding concentration, adding concentration is 0.3% o'clock, and frictional coefficient and wear scar diameter reach minimum value.
As can be seen from Figure 7, under the condition that straight lubrication oil lubricates, wear scar diameter is bigger, and mill spot surface ratio is more coarse, and ditch dug with a plow is darker, and the scratch degree is more serious, and this moment, the degree of wear was comparatively serious.
Obviously find out at the wear scar diameter that steel ball under the lubricated condition of oleophilic metal sulfide is arranged little manyly under obviously than straight lubrication oil lubricating condition from Fig. 8 and Fig. 9, and surface of friction pair is smooth, and ditch dug with a plow is more shallow, and the scratch degree is lighter.This is mainly with to contain a large amount of oil loving nano metal sulfide particle grains relevant in the lubricating oil, in friction process, nano particle and friction surface generation friction chemical reaction, can between friction pair, form firm lubricant film, make it become more smooth to friction surface reparation, thereby play wear-resistant effect.
Therefore, the oil loving nano metal sulphide of institute's synthetic of the present invention can effectively improve the antiwear and antifriction ability of lubricating oil.

Claims (5)

1. the preparation method of a nano lubricating fluid comprising oleophilic metal sulfide is characterized in that:
A) preparation of organic metal salt presoma
Step 1 joins the mixed solvent of normal hexane and dehydrated alcohol in the reaction vessel, and then to add reaction raw materials 1 concentration range be the copper chloride solution of 0.5~2mol/L, and wherein three's volume ratio is 7: 4: 3;
Step 2 joins reaction raw materials 2 sodium oleates in the above-mentioned reaction vessel, and wherein the mol ratio of cupric chloride and sodium oleate is 1: 2, reacts 2~5h under 65~85 ℃ heating condition;
Step 3, reaction is isolated inorganic phase and organic phase after finishing from reaction solution, and washs more than three times with deionized water to organic phase;
Step 4 at 3~20KPa, is carried out underpressure distillation under 50~60 ℃ of conditions to organic phase, removes organic solvent and obtains the organic metal salt presoma;
B) original position of oleophilic metal sulfide is synthetic
Step 1 joins above-mentioned organic metal salt presoma and coating materials oleic acid in another reaction vessel, and both mol ratios are 1: 2~2: 1;
Step 2 adds lubricating oil as reaction medium again in reaction vessel, wherein the content of organic metal salt presoma in lubricating oil is 0.1~1mol/Kg;
Step 3, the material in the reacting by heating container also keeps 25~35 ℃, is stirred to the organic metal salt presoma and is dissolved in the lubricating oil fully;
Step 4 slowly feeds the exsiccant hydrogen sulfide in reaction vessel, under 25~45 ℃ of temperature of reaction, continue stirring reaction 2~4h, and promptly obtaining concentration is w 1The mother liquor that contains the oleophilic metal sulfide nano particle, w 1Scope be 1.00~10.0%;
w 1 = M × n W × 100 %
Wherein M is the formula weight of metallic sulfide; N is the amount of substance of metallic sulfide, unit: mol; W is the quality of lubricating oil, unit: g;
C) preparation of nano lubricating fluid
With quality is m 1Above-mentioned mother liquor and quality be m 2Lubricating oil be in harmonious proportion stirring, promptly obtaining concentration is w 2Nano lubricating fluid, w 2Scope be 0.05~3.00%, determine the add-on m of lubricating oil according to following formula 2
m 2 = ( w 1 - w 2 ) × m 1 w 2 .
2. the preparation method of a kind of nano lubricating fluid comprising oleophilic metal sulfide according to claim 1, it is characterized in that the described mixed solvent of step 1 in the preparation of organic metal salt presoma uses the mixed solvent of normal heptane and dehydrated alcohol, its volume ratio is 7: 4.
3. the preparation method of a kind of nano lubricating fluid comprising oleophilic metal sulfide according to claim 1, it is characterized in that the described reaction raw materials 1 of step 1 in the preparation of organic metal salt presoma uses the aqueous solution of copper sulfate, cupric nitrate, neutralized verdigris, nickelous chloride, single nickel salt, zinc chloride, zinc sulfate, zinc nitrate, zinc acetate, lead chloride, lead nitrate or plumbic acetate, its concentration range is 0.5~2mol/L.
4. the preparation method of a kind of nano lubricating fluid comprising oleophilic metal sulfide according to claim 1 is characterized in that the described reaction raw materials 2 of step 2 uses potassium oleates in the preparation of organic metal salt presoma.
5. the preparation method of a kind of nano lubricating fluid comprising oleophilic metal sulfide according to claim 1 is characterized in that the synthetic middle described lubricating oil of step 2 of original position of oleophilic metal sulfide is meant cut lubricating oil, hydro carbons lubricating oil, polyether class lubricating oil or silicone oil lubricating oil.
CNB2005101302584A 2005-12-15 2005-12-15 Method for preparing nano lubricating fluid comprising oleophilic metal sulfide Expired - Fee Related CN100334187C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CNB2005101302584A CN100334187C (en) 2005-12-15 2005-12-15 Method for preparing nano lubricating fluid comprising oleophilic metal sulfide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CNB2005101302584A CN100334187C (en) 2005-12-15 2005-12-15 Method for preparing nano lubricating fluid comprising oleophilic metal sulfide

Publications (2)

Publication Number Publication Date
CN1775933A CN1775933A (en) 2006-05-24
CN100334187C true CN100334187C (en) 2007-08-29

Family

ID=36765655

Family Applications (1)

Application Number Title Priority Date Filing Date
CNB2005101302584A Expired - Fee Related CN100334187C (en) 2005-12-15 2005-12-15 Method for preparing nano lubricating fluid comprising oleophilic metal sulfide

Country Status (1)

Country Link
CN (1) CN100334187C (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ITUB20156248A1 (en) * 2015-12-04 2017-06-04 Alpha Biopesticides Ltd ? COMPOSITION FOR CROP CARE AND PROTECTION? (? COMPOSITION FOR CARE AND PROTECTION OF CULTIVATIONS?)
CN115404115B (en) * 2022-08-30 2023-09-15 河南大学 Nano copper lubricating oil additive and preparation method thereof
CN115786027B (en) * 2022-12-14 2024-01-12 中国科学院兰州化学物理研究所 Water-based microemulsified cutting fluid

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1221748A (en) * 1998-08-28 1999-07-07 中国科学院兰州化学物理研究所 Sulphur-containing organic compound modified metal-chalocogenide nm particles, its prepn. and application
CN1400297A (en) * 2001-07-31 2003-03-05 中国科学院兰州化学物理研究所 Synthesis method of nano sulfur compound capable of stably dispersing in oil medium
CN1468945A (en) * 2003-07-02 2004-01-21 清华大学 Prepn of oil dispersed molybdenum disulfide
CN1611543A (en) * 2003-10-30 2005-05-04 中国人民解放军后勤工程学院 Heavy polymer / chalcogenide nano composite material in situ preparing method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1221748A (en) * 1998-08-28 1999-07-07 中国科学院兰州化学物理研究所 Sulphur-containing organic compound modified metal-chalocogenide nm particles, its prepn. and application
CN1400297A (en) * 2001-07-31 2003-03-05 中国科学院兰州化学物理研究所 Synthesis method of nano sulfur compound capable of stably dispersing in oil medium
CN1468945A (en) * 2003-07-02 2004-01-21 清华大学 Prepn of oil dispersed molybdenum disulfide
CN1611543A (en) * 2003-10-30 2005-05-04 中国人民解放军后勤工程学院 Heavy polymer / chalcogenide nano composite material in situ preparing method

Also Published As

Publication number Publication date
CN1775933A (en) 2006-05-24

Similar Documents

Publication Publication Date Title
Song et al. Synthesis of monodispersed ZnAl2O4 nanoparticles and their tribology properties as lubricant additives
CN105316077B (en) A kind of graphene/nitridation carbon quantum dot composite nano materials and lubricating oil friction modifier
CN104593132B (en) Metalworking fluid of graphene-containing dispersion liquid and preparation method thereof
CN105647612B (en) A kind of lubricating grease containing nano-carbon material and preparation method thereof
CN103073060B (en) Method for preparing hexagonal molybdenum disulfide nanosheet as anti-friction additive
CN102807907B (en) Graphene/metal oxide semiconductor (MoS2) nano self-lubricating composite material and preparation method thereof
US20130079262A1 (en) Novel materials as additives for advanced lubrication
CN107557110A (en) A kind of preparation method of molybdenum disulfide nano sheet load nano copper particle lubriation material
Huang et al. Friction and wear properties of IF–MoS 2 as additive in paraffin oil
CN106381190A (en) A graphitic carbon nitride-molybdenum disulfide composite nano-material, a preparing method thereof and uses of the nano-material
Lingtong et al. Synthesis and surface modification of the nanoscale cerium borate as lubricant additive
CN100334187C (en) Method for preparing nano lubricating fluid comprising oleophilic metal sulfide
CN104194863A (en) Preparation method of nano copper@titanium dioxide core-shell structure lubricating oil additive
CN110564378B (en) Environment-friendly lubricant for drilling fluid and preparation method and application thereof
WO2019076196A1 (en) Graphene/trimanganese tetraoxide composite nano lubricating additive and synthesis method thereof
Zhang et al. Thiadiazole functionalized covalent organic frameworks as oil-based lubricant additives for anti-friction and anti-wear
CN108017939B (en) Thiadiazole derivative modified graphene and preparation method and application thereof
Wang et al. Interface synthesis for controllable construction of 2D Zn (Bim)(OAc) nanosheets via oil/water system and their application in oil
Zhang et al. Tribochemical synthesis of functionalized covalent organic frameworks for anti-wear and friction reduction
Yang et al. Branch-chain length modulated graphene oxides for regulating the physicochemical and tribophysical properties of pickering emulsions
CN110041985B (en) Composite nano lubricating oil additive with self-repairing function and preparation method thereof
Zhu et al. One-pot synthesis for 2D nanostructured calcium borate/Ni-BDC composite nanosheets enabled tribological improvement
CN115353922A (en) Carbon nitride quantum dot-based polyethylene glycol lubricating additive and preparation method thereof
CN105950260A (en) Method for obtaining lubricating oil containing lubrication-friendly MoS2 nano-particles
Ye et al. Mechanochemical in-situ construction of ionic liquid-functionalized covalent organic frameworks for anti-wear and friction reduction

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20070829

Termination date: 20100115