CN102229839A - Method for preparing modified nano zinc borate antiwear agent and method for dispersing modified nano zinc borate antiwear agent in base oil - Google Patents
Method for preparing modified nano zinc borate antiwear agent and method for dispersing modified nano zinc borate antiwear agent in base oil Download PDFInfo
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- CN102229839A CN102229839A CN2011101394666A CN201110139466A CN102229839A CN 102229839 A CN102229839 A CN 102229839A CN 2011101394666 A CN2011101394666 A CN 2011101394666A CN 201110139466 A CN201110139466 A CN 201110139466A CN 102229839 A CN102229839 A CN 102229839A
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Abstract
The invention relates to a method for preparing a modified nano zinc borate antiwear agent and a method for dispersing the modified nano zinc borate antiwear agent in base oil. The method for preparing the modified nano zinc borate antiwear agent comprises: uniformly mixing borax and water according to a mass ratio, and uniformly mixing zinc nitrate and ethanol according to a mass ratio; dripping oleic acid into solution of borax, and continuously stirring for 1 to 5 hours at a temperature of 40 to 80 DEG C and at a rotation speed of 200 to 900 r/min; dropwise dripping the ethanol solution of zinc nitrate into borax solution into which oleic acid is dripped, stirring, cooling, filtering and obtaining the product; and adding the product of filtration into ethanol, stirring to obtain suspension, standing the suspension for 15 to 60 minutes and collecting supernate. A new quick evaporation method comprises: dropwise dripping the obtained supernate into the base oil at a temperature of 90 to 140 DEG C, wherein the mass ratio of the base oil to the supernate is 1:(1-5); and stirring at a speed of 200 to 800r/min and obtaining the base oil in which the nano zinc borate is dispersed uniformly. The dispersion of the nano zinc borate by the quick evaporation method is more uniform, and the agglomeration appeared in the conventional method is avoided.
Description
Technical field
The present invention relates to a kind of preparation and dispersing method thereof of lubricating oil additive, the particularly preparation method of modified Nano zinc borate anti-wear agent and dispersing method in base oil.
Background technology
Lubricating oil is industrial now blood, and lubricating oil additive then is the marrow of various senior lubricants, is the key that improves lubricity.Lubricating oil additive is a main ingredient of guaranteeing quality of lubrication oil, though in lubricating oil the amount ratio base oil much less of additive, its importance and not second to base oil, even be higher than base oil.The purpose of using lubricating oil is exactly the friction and wear that is used for reducing machinery, improves mechanical efficiency, cuts down the consumption of energy, and prevents sintering, the prolonged mechanical life-span.And the lubricating oil additive that anti-wear agent arises at the historic moment just thereupon, wearing and tearing are used for reducing friction.
Anti-wear agent occupies critical role as one of 5 big additives of modern lubricating oil in lubricating oil additive, the research and development of its product innovation also are in the prostatitis of modern lubricating oil development always.And traditional lubrication oil antiwear agent is owing to contain P and S and can make three-way catalyst in the tail gas convertor poison, influence accuracy that oxygen sensor measures to reach toxicity to ecotope, particularly world regulation traditional anti-wear agent of phosphorus, sulphur class is limited the quantity of use and situation that working condition requirement is harsh day by day under, the development of traditional anti-wear agent has run into bottleneck.
But continuous development along with nano material and Nanotribology, in recent years, Chinese scholars has turned to nano material with attention gradually in the process of the lubricating oil additive of the excellent abrasion resistance of exploitation, and it has been carried out a series of Study on Friction Properties, obtained good effect.Such as the nano boric acid cerium in the nano boric acid salt, the boric acid cerium has good wear resistance.But the borate as anti-wear agent has a fatal weakness, is difficult to dissolving and stable dispersion in oil, and this has also limited it in industrial widespread adoption.Because its difficulty in oil is disperseed, so boratory scattering problem becomes the key of nano boric acid salt anti-wear agent abrasion resistance.
Summary of the invention
The object of the present invention is to provide a kind of modification the nano-zinc borate anti-wear agent the preparation method and this nano-zinc borate is dispersed in a kind of novel method in the base oil as additive.
For achieving the above object, the present invention is achieved through the following technical solutions:
The preparation method of a kind of modified Nano zinc borate anti-wear agent of the present invention, step is as follows:
1) is 1: 20～60 to mix borax and water according to mass ratio, zinc nitrate and ethanol are mixed according to mass ratio 1: 10～40;
2) Jiang oleic acid is added drop-wise to 1) in the described borax soln, be that 40～80 ℃ and rotating speed are 200～900 rev/mins and continue down to stir 1～5 hours in temperature;
3) with 1) in make zinc nitrate ethanolic soln dropwise join 2 by 11～140ml volume) in the mixed solution that obtained, stirred 0.5～5 hour; Cooled and filtered gets product;
4) with 3) the product water and the ethanol of gained washes respectively, filters products therefrom then and joins and stir into the suspension state in the ethanol, leaves standstill this suspension 15～60 minutes, gets supernatant liquid.
Described borax, zinc nitrate, oleic acid all are analytical pure, three's ratio of quality and the number of copies 5: 3～6: 8～12.Preferred mass portion rate 5: 4～5: 9～10.
Modified Nano zinc borate anti-wear agent of the present invention dispersing method in base oil, use novel rapid evaporation method: it is in 90～140 ℃ the base oil that the supernatant liquid of gained is dropwise joined temperature, the mass ratio of base oil and supernatant liquid is 1: 1～5, and stir 200～800 rev/mins speed, obtain the finely dispersed base oil of nano-zinc borate.
Preferred temperature is 100～135 ℃ in the above-mentioned dispersing method, and rotating speed is 400-600 rev/min, and the preferable range of the mass ratio of base oil and supernatant liquid is 1: 2～3.
The present invention uses the rapid evaporation method that nano-zinc borate is scattered in the base oil, and manufacturing process is grasped control easily, and cost is low.And the nano-zinc borate that obtains with respect to traditional method, the nano-zinc borate dispersive that uses rapid evaporation method gained is (as Fig. 1) more evenly, the agglomeration as traditional method (as Fig. 2) do not occur.
Description of drawings
Fig. 1: rapid evaporation method gained nano-zinc borate particulate electromicroscopic photograph of the present invention;
Fig. 2: traditional method gained nano-zinc borate particulate electromicroscopic photograph.
Embodiment
Embodiment 1
The 1.50g borax is dissolved in 24ml (about 24g) water, and the 0.90g zinc nitrate is dissolved in 11ml (about 9g) ethanol.The oleic acid of 2ml (about 2.4g) joins in the mixing solutions of borax, is heated to 40 ℃ and be under 200 rev/mins at rotating speed, mechanical stirring 1 hour.The alcoholic solution 11ml of zinc nitrate dropwise put to be added to be dissolved in the boric acid solution, constant temperature stirs.0.5 cold filtration after hour.Water and ethanol clean respectively four times, with filter to clean the back gained product be dissolved in the 80ml ethanol, stir into suspension, left standstill 15 minutes.Used borax, zinc nitrate, oleic ratio of quality and the number of copies are 5: 3: 8.
Getting supernatant liquid, to join temperature be 90 ℃, and quality is in the base oil of 20g, and with 500 rev/mins rotating speed, and what obtain that the rapid evaporation method makes is dispersed in nano-zinc borate particle in the base oil;
Embodiment 2
The 2.20g borax is dissolved in 130ml (about 130g) water, and the 2.6g zinc nitrate is dissolved in 130ml (about 104g) ethanol.The oleic acid of 6ml (about 5.28g) joins in the mixing solutions of borax, is heated to 60 ℃ and be under 500 rev/mins at rotating speed, mechanical stirring 2 hours.The alcoholic solution 130ml of zinc nitrate dropwise put to be added to be dissolved in the boric acid solution, constant temperature stirs cold filtration after 3 hours.Water and ethanol clean respectively four times, with filter to clean the back gained product be dissolved in the 100ml ethanol, stir into suspension, left standstill 20 minutes.Used borax, zinc nitrate, oleic ratio of quality and the number of copies are 5: 6: 12.
Getting supernatant liquid, to join temperature be 100 ℃, and quality is in the base oil of 30g, and with 300 rev/mins rotating speed, and what obtain that the rapid evaporation method makes is dispersed in nano-zinc borate particle in the base oil;
Get the supernatant liquid filtration and obtain the nano-zinc borate particle, get 0.2g nano-zinc borate particle and join in the 40g base oil at 125 ℃ of vacuum dryings; With mixture ultrasonic vibration 1 hour under 60 ℃ of temperature, after ultrasonic the finishing with base oil and zinc borate mixed solution mechanical stirring 2 hours; Can obtain the base oil that contains nano-zinc borate that traditional law system gets.
Get the comparative example of example 2 as traditional method and rapid evaporation method.When adding base oil massfraction 1% zinc borate in the basis has, the actual mass mark of the zinc borate that traditional method obtains is 0.25%, and the actual mass mark of the zinc borate that obtains of rapid evaporation method is 0.9%, very near 1% addition.Illustrate and use the rapid evaporation method all to dissolve, use traditional method then the part in the zinc borate that adds can only to be dissolved in the base oil almost all adding the zinc borate that advances base oil.By more as can be seen, the rapid evaporation method is better than traditional method.
Embodiment 3
The 3g borax is dissolved in 90ml (about 90g) water, and the 3g zinc nitrate is dissolved in 75ml (about 60g) ethanol.The oleic acid of 6ml (about 5.4g) joins in the mixing solutions of borax, is heated to 70 ℃ and be under 700 rev/mins at rotating speed, mechanical stirring 4 hours.The alcoholic solution 75ml of zinc nitrate dropwise put to be added to be dissolved in the boric acid solution, constant temperature stirs cold filtration after 2 hours.Water and ethanol clean respectively four times, with filter to clean the back gained product be dissolved in the 120ml ethanol, stir into suspension, left standstill 30 minutes.Used borax, zinc nitrate, oleic ratio of quality and the number of copies are 5: 5: 9.
Getting supernatant liquid, to join temperature be 110 ℃, and quality is in the base oil of 50g, and with 450 rev/mins rotating speed, and what obtain that the rapid evaporation method makes is dispersed in nano-zinc borate particle in the base oil;
Get the supernatant liquid filtration and obtain the nano-zinc borate particle, get 0.25g nano-zinc borate particle and join in the 35g base oil at 130 ℃ of vacuum dryings; With mixture ultrasonic vibration 2 hours under 65 ℃ of temperature, after ultrasonic the finishing with base oil and zinc borate mixed solution mechanical stirring 3 hours; Can obtain the base oil that contains nano-zinc borate that traditional law system gets.
Embodiment 4
The 3.50g borax is dissolved in 105ml (about 105g) water, and the 2.8g zinc nitrate is dissolved in 140ml (about 112g) ethanol.The oleic acid of 8ml (about 7g) joins in the mixing solutions of borax, is heated to 80 ℃ and be under 900 rev/mins at rotating speed, mechanical stirring 5 hours.The alcoholic solution 140ml of zinc nitrate dropwise put to be added to be dissolved in the boric acid solution, constant temperature stirs cold filtration after 5 hours.Water and ethanol clean respectively four times, with filter to clean the back gained product be dissolved in the 150ml ethanol, stir into suspension, left standstill 60 minutes.Used borax, zinc nitrate, oleic ratio of quality and the number of copies are 5: 4: 10.
Getting supernatant liquid, to join temperature be 100 ℃, and quality is in the base oil of 60g, and with 700 rev/mins rotating speed, and what obtain that the rapid evaporation method makes is dispersed in nano-zinc borate particle in the base oil;
Get the supernatant liquid filtration and obtain the nano-zinc borate particle, get 0.3g nano-zinc borate particle and join in the 40g base oil at 140 ℃ of vacuum dryings; With mixture ultrasonic vibration 1.5 hours under 70 ℃ of temperature, after ultrasonic the finishing with base oil and zinc borate mixed solution mechanical stirring 5 hours; Can obtain the base oil that contains nano-zinc borate that traditional law system gets.
The rapid evaporation method of the technical characterictic in the scope of the invention and traditional method relatively use the nano-zinc borate dispersive of rapid evaporation method gained more even, the agglomeration as the traditional method do not occur.
Claims (5)
1. the preparation method of a modified Nano zinc borate anti-wear agent is characterized in that step is as follows:
1) is 1: 20～60 to mix borax and water according to mass ratio, zinc nitrate and ethanol are mixed according to mass ratio 1: 10～40;
2) Jiang oleic acid is added drop-wise to 1) in the described borax soln, be that 40～80 ℃ and rotating speed are 200～900 rev/mins and continue down to stir 1～5 hours in temperature;
3) with 1) in make zinc nitrate ethanolic soln dropwise join 2 by 11～140ml volume) in the mixed solution that obtained, stirred 0.5～5 hour; Cooled and filtered gets product;
4) with 3) the product water and the ethanol of gained washes respectively, filters products therefrom then and joins and stir into the suspension state in the ethanol, leaves standstill this suspension 15～60 minutes, gets supernatant liquid.
2. modified Nano zinc borate anti-wear agent preparation method as claimed in claim 1 is characterized in that described borax, zinc nitrate, oleic acid all are analytical pure, three's ratio of quality and the number of copies 5: 3～6: 8～12.
3. modified Nano zinc borate anti-wear agent preparation method as claimed in claim 2 is characterized in that described ratio of quality and the number of copies 5: 4～5: 9～10.
4. modified Nano zinc borate anti-wear agent dispersing method in base oil of claim 1 is characterized in that using novel rapid evaporation method: it is in 90～140 ℃ the base oil that the supernatant liquid of gained is dropwise joined temperature; The mass ratio of base oil and supernatant liquid is 1: 1～5, and stirs 200～800 rev/mins speed, obtains the finely dispersed base oil of nano-zinc borate.
5. dispersing method as claimed in claim 4 is characterized in that temperature is 100～135 ℃, and rotating speed is 400-600 rev/min, and base oil is 1: 2～3 with the quality of supernatant liquid than scope.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633277A (en) * | 2012-05-02 | 2012-08-15 | 天津大学 | Preparation method of synergistic flame retardant nanometer zinc borate |
| CN102925251A (en) * | 2012-11-27 | 2013-02-13 | 沈阳工业大学 | Method for preparing nano-borate particles in liquid-state lubricating oil |
| WO2021221582A1 (en) * | 2020-04-28 | 2021-11-04 | Celal Bayar Universitesi Tekn. Gel. Bol. A. S. | Production of metal borates with nano-dimension |
| CN114774183A (en) * | 2022-05-10 | 2022-07-22 | 扬州大学 | Zinc borate/Fe-BDC nano composite lubricating oil additive and preparation method thereof |
-
2011
- 2011-05-26 CN CN2011101394666A patent/CN102229839A/en active Pending
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633277A (en) * | 2012-05-02 | 2012-08-15 | 天津大学 | Preparation method of synergistic flame retardant nanometer zinc borate |
| CN102925251A (en) * | 2012-11-27 | 2013-02-13 | 沈阳工业大学 | Method for preparing nano-borate particles in liquid-state lubricating oil |
| WO2021221582A1 (en) * | 2020-04-28 | 2021-11-04 | Celal Bayar Universitesi Tekn. Gel. Bol. A. S. | Production of metal borates with nano-dimension |
| CN114774183A (en) * | 2022-05-10 | 2022-07-22 | 扬州大学 | Zinc borate/Fe-BDC nano composite lubricating oil additive and preparation method thereof |
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Application publication date: 20111102 |