CN102191118B - Oil-based suspended base liquid of nano diamond powder and preparation process thereof - Google Patents
Oil-based suspended base liquid of nano diamond powder and preparation process thereof Download PDFInfo
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- CN102191118B CN102191118B CN 201110087009 CN201110087009A CN102191118B CN 102191118 B CN102191118 B CN 102191118B CN 201110087009 CN201110087009 CN 201110087009 CN 201110087009 A CN201110087009 A CN 201110087009A CN 102191118 B CN102191118 B CN 102191118B
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Abstract
The invention relates to oil-based suspended base liquid of nano diamond powder and a preparation process thereof, and belongs to the technical field of additives of abrasives and lubricating oil. The preparation process is characterized by comprising the following steps of: performing high-temperature treatment on the nano diamond powder; grinding and crushing the nano diamond powder; wetting and wrapping the nano diamond particles by using a nonionic surfactant; and dispersing and isolating the nano diamond particles into base oil by using an amide type oil-soluble dispersing agent, wherein the used surfactant and the dispersing agent do not comprise elements except carbon, hydrogen, oxygen and nitrogen.
Description
Technical field
The invention belongs to abrasive, lubricating oil additive technical field, particularly a kind of development of oil base suspension base fluid of nano-diamond powder.
Background technology
Nano diamond itself belongs to a kind of ultra micro superhard material, in polishing, grinds, and the aspects such as resistance to compression all are widely used.But size is little, specific surface area is large and specific surface energy is high because Nano diamond usually forms under the High Temperature High Pressure under the detonation state, has, and very easily reunites, thereby has limited its widespread use.Therefore, realizing the stable dispersion of Nano diamond, is that Detonation Process prepares one of later stage important application direction of Nano diamond.
Dispersion for nano-diamond powder, there are at present a lot of documents and patent all to carry out the research of this respect, investigators such as Russia JSC research centre directly are scattered in Nano diamond in the water, obtained the diamond suspension (L.V.Agibalova of the about 300nm of mean sizes, A.P.Voznyakovskii, V.Yu.Dolmatov.Structure of suspensions of explosion-synthesized ultradispersed diamonds.Superhard Materials, 1998, (4): 79-87.); For another example Chiganova. (G.A.Chiganova, V.A.Boonger, A.S.Chiganov.Electrophoretic technology of hydrosols of ultradispersed diamond and modification of its surface[J] .Colloid is J.1993,55 (5): 774-775.) etc., contain the diamond aqueous solution of aluminum chloride by heating, obtained the water-based diamond suspension of the about hundreds of nanometer of dispersion size; Domestic research such as Zhang Dong (Zhang Dong, Tong Yi, yellow wind thunder.The research of detonation Nano diamond dispersiveness in ethanol, nanometer processing technique.2005,2 (6): 46-49.) etc., the employing high molecular polymer is that dispersion agent, dehydrated alcohol are made solvent, ultrasonicly tested as the dispersion means, has obtained the diamond colloidal solution of median size 51.7nm, can the about 80min of stable dispersion.The patent of this respect such as patent (application number: 200810041820.X, China .) prepared nanometer alcohol diamond fluid, wherein diamond content is about 0.1%-5% (volume content), the method is at first with the Nano diamond surface hydroxylation, then disperse in stirring and ultrasonic situation with alcohols material, diamond particle size is about 1000nm in the fluid for preparing.Patent (application number: 200780025959.9, Chinese) and patent (application number: 200880107513.5, China) at first Nano diamond is fluoridized, then directly mix with alcohols, having made can stable dispersion 120h, and size is about the diamond dispersion liquid of 10-300nm.Owing to be that the Nano diamond powder directly is scattered in the ethanol, very easily occur between the particle again to bond and reunite, so the stable suspersion time is not long in these class methods.
Therefore, nano-powder is disperseed, if adopt merely mechanical means, the hard aggregation between nanoparticle that also can dissociate can keep stable for a long time but be difficult to guarantee system; And if only adopt chemical process to process, as adding inorganic electrolyte or tensio-active agent etc. medium and powder are carried out modification, same being difficult to carrying out depolymerization in conjunction with polymer firmly between particle.Based on this, the present invention is carrying out adding tensio-active agent when brute force is dissociated to agglomeration Nano diamond powder, thereby effectively stops nano-powder again to bond and reunite, and guarantees effective dispersion of nano-powder.This respect is similarly studied such as patent (application number: 200910069723.6, China) in ethanol medium, adopt the zirconium dioxide microballoon to grind 2～5 hours polytetrafluorethylepowder powder and Nano diamond powder, obtain nanodiamond liquid dispersion, then add polyether-ether-ketone and polytetrafluorethylepowder powder, the oven dry compacting is again through sinter molding, this patent uses polyvinylpyrrolidone as dispersion agent, diamond content is 0.5～2.0% in the dispersion liquid that makes, mean particle size is less than 20nm, but only limits to Nano diamond is scattered in the solid.Patent (application number: 200910227674.4, China) after dispersion agent (siliceous alkyl aryl polyether) grinds, adds auxiliary with Nano diamond, prepared diamond content and be 0.3% dispersion liquid; Patent (application number: 01131537.7, China) a kind of dispersing technology of Nano diamond has been proposed, adopt aluminum stearate, trisodium phosphate, Sodium dodecylbenzene sulfonate and other tensio-active agent, by ultrasonic technology, nanoparticle is scattered in the lubricating oil, diamond content is 1%～10%.The shortcoming of such dispersing method is, contains aluminium, silicon, zinc in auxiliary or the dispersion agent, sulphur, and phosphorus, the elements such as sodium produce impurity and toxic side effect easily, and equipment is produced corrosion.
The nano-diamond powder that adopts among the present invention is detonation synthesis, wherein contains the materials such as graphite-phase, decolorizing carbon, and wherein particle surface has hydrophilic group, as-OH ,-COOH ,-NH
2Deng; The present invention utilizes this hydrophilic characteristics, Nano diamond powder coacervate is carried out brute force to be disperseed, and adopt non-ionic water-soluble tensio-active agent and acid amide type oil-soluble dispersant that its surface is coated, realize that stable dispersion in base oil, has obtained diamond content and has been about 10%～14% oil base suspension base fluid.
Summary of the invention
The nano-diamond powder that detonation is synthetic, the premium properties of itself is owing to the factors such as its reunion can not get bringing into play fully and using.Problem to be solved by this invention is to reunite in order to overcome the Nano diamond powder, and makes it stable dispersion in lubricating base oil, to improve friction resistant and the extreme pressure property of base oil (lubricating oil).
Technical scheme of the present invention is: at first high temperature is removed part surplus carbon and other impurity in the powder, then by shredder after brute force is opened powder reuniting under the ethanol medium, add nonionic surface active agent and dispersion agent, make it to be coated on nano powder surface, thereby the prevention powder bonds again and reunites.
Nano-diamond powder of the present invention is the carbon dust of detonation synthesis, wherein contains diamond, graphite-phase, and decolorizing carbon etc., wherein particle surface has hydrophilic radical, as-OH ,-COOH ,-NH
2Deng; These groups can with some tensio-active agent and dispersion agent generation coupling reaction, make it be coated on the nano-powder particle surface.Among the present invention, main use does not contain de-carbon, and hydrogen, the nonionic surface active agent of the element outside oxygen, the nitrogen carry out wetting to the Nano diamond particle and coats, then with its dispersion be isolated from the base oil.
Among the present invention, the weight percent of nano-diamond powder, surfactant A, surfactant B, basic wet goods composition is:
Nano-diamond powder: 10～14%;
Surfactant A: 10～14%;
Surfactant B: 50～70%;
Base oil: less than 10%;
Described surfactant A is not for containing de-carbon, hydrogen, the non-ionic water-soluble tensio-active agent of element outside oxygen, the nitrogen;
Described surfactant B is not for containing de-carbon, hydrogen, the acid amide type oil-soluble dispersant of element outside oxygen, the nitrogen.
This suspension is preparation technology mainly may further comprise the steps:
1. nano-diamond powder is placed air atmosphere, 400 ℃ of lower high-temperature heat treatment 1h;
2. cool off under drying regime until the nano-diamond powder after the pyroprocessing, grind after the abundant wetting mixing of adding ethanol, obtain the alcohol suspension of Nano diamond powder;
3. remove larger particles and other impurity in the Nano diamond powder alcohol suspension of gained;
4. add surfactant A at Nano diamond powder alcohol suspension according to a certain percentage, surfactant B and base oil are being no more than heating under vacuum under 100 ℃ of temperature, and ultrasonic wave is disperseed simultaneously, oven dry ethanol; Make the oil base suspension base fluid of nano-diamond powder.
The suspension base fluid that the present invention prepares can be good be scattered in the lubricating oil; The particle median size of nano-powder in the suspension base fluid is 30nm～100nm, and the particle distribution scope is 20nm～130nm; Solution keeps clear when being diluted to diamond quality content and being 0.01%～0.5%, under static state can keep at least not precipitating in 3 months.Employed tensio-active agent and dispersion agent be sulfur-bearing not all, the perishable easy toxigenous elements such as phosphorus, chlorine, fluorine and metallic element.It is simple that this technology has technique, easy to operate, and nontoxic pair is without characteristics such as corrosion.
Description of drawings
Fig. 1 is the oil base suspension base fluid finished product synoptic diagram of nano-diamond powder of the present invention.
Fig. 2 is that the oil base suspension base fluid of nano-diamond powder of the present invention is diluted in synoptic diagram behind the base oil.
Fig. 3 is the particle size distribution figure after the oil base suspension base fluid of nano-diamond powder of the present invention is diluted in base oil.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme and accompanying drawing.
Embodiment 1
1. get the certain mass nano-diamond powder, insert in the retort furnace, adjust the temperature to 400 ℃, roasting 1 hour;
2. baked sample is cooled off under drying regime, add ethanol, fully wetting being placed in the sand mill starts the machine, and adjusting rotary speed constantly adds ethanol to 2000r/min in the circular grinding process;
3. behind the 1h, discharging.Filter impurity, and under the rotating speed of 4000r/min centrifugal rotation 5min, remove wherein and stir behind the larger particles, take out 10ml powder (a), and determine simultaneously residue powder volume (b); Remove ethanol among a, determine wherein nano-powder quality, and then nano-powder quality among definite b.
4. according to
Powder: 1
OP-10 (surfactant A): 1
Diene base polyisobutenyl succimide (surfactant B): 8
Ratio (mass ratio) adds surfactant A, surfactant B, and be no more than heating under vacuum under 100 ℃ of temperature, ultrasonic wave is disperseed simultaneously, oven dry ethanol; Namely get this oil base suspension base fluid, the Nano diamond powder content is 10%.
Embodiment 2
1. 2. 3. with case one;
4. according to
Powder: 1
OP-10 (surfactant A): 1
Diene base polyisobutenyl succimide (surfactant B): 5
Ratio (mass ratio) adds surfactant A, surfactant B, and be no more than heating under vacuum under 100 ℃ of temperature, ultrasonic wave is disperseed simultaneously, oven dry ethanol; Namely get this oil base suspension base fluid, the Nano diamond powder content is 14.28%.
Embodiment 3
1. 2. 3. with case one;
4. according to
Ratio (mass ratio) adds surfactant A, surfactant B, and be no more than heating under vacuum under 100 ℃ of temperature, ultrasonic wave is disperseed simultaneously, oven dry ethanol; Namely get this oil base suspension base fluid, the Nano diamond powder content is 12.5%.
Claims (1)
1. the oil base suspension base fluid of a nano-diamond powder is characterized in that, this oil base suspension base fluid is comprised of nano-diamond powder, surfactant A, surfactant B, base oil, and the weight percent of each composition is:
Nano-diamond powder: 10～14%; Surfactant A: 10～14%; Surfactant B: 50～70%;
Base oil: less than 10%; Each component content sum is 100%;
Described nano-diamond powder is the carbon dust of detonation synthesis;
Described surfactant A is not for containing de-carbon, hydrogen, oxygen, the non-ionic water-soluble tensio-active agent of element outside the nitrogen;
Described surfactant B is not for containing de-carbon, hydrogen, oxygen, the acid amide type oil-soluble dispersant of element outside the nitrogen;
The preparation technology of above-mentioned oil base suspension base fluid may further comprise the steps:
1. nano-diamond powder is placed air atmosphere, 400 ℃ of lower high-temperature heat treatment 1h;
2. cool off under drying regime until the nano-diamond powder after the pyroprocessing, grind after the abundant wetting mixing of adding ethanol, obtain the alcohol suspension of Nano diamond powder;
3. remove larger particles and other impurity in the Nano diamond powder alcohol suspension of gained;
4. add surfactant A in described ratio at Nano diamond powder alcohol suspension, surfactant B and base oil are being no more than heating under vacuum under 100 ℃ of temperature, and ultrasonic wave is disperseed simultaneously, dry ethanol, make the oil base suspension base fluid of nano-diamond powder.
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| CN 201110087009 CN102191118B (en) | 2011-04-07 | 2011-04-07 | Oil-based suspended base liquid of nano diamond powder and preparation process thereof |
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| CN 201110087009 CN102191118B (en) | 2011-04-07 | 2011-04-07 | Oil-based suspended base liquid of nano diamond powder and preparation process thereof |
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| CN102191118B true CN102191118B (en) | 2013-01-30 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103131528B (en) * | 2013-02-08 | 2014-10-08 | 浣石 | Nano-diamond-containing water base lubricating fluid and preparation method thereof |
| CN103773553B (en) * | 2013-11-29 | 2015-04-01 | 福建六九环保科技有限公司 | Nano-diamond lubricant additive as well as formula, production process and application thereof |
| CN103923724B (en) * | 2014-04-24 | 2016-03-02 | 重庆海立云科技有限公司 | The automatic repair liquid of Nano diamond for piston engine |
| CN106479598A (en) * | 2016-03-09 | 2017-03-08 | 天津迪麦爱科科技有限公司 | A kind of engine lubricating oil additive containing Nano diamond |
| CN111676084A (en) * | 2020-06-19 | 2020-09-18 | 大连理工大学重大装备设计与制造郑州研究院 | Environment-friendly type cubic press ultrahigh pressure working circulating liquid and preparation method thereof |
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| CN1331581C (en) * | 2004-05-14 | 2007-08-15 | 深圳市金刚源新材料发展有限公司 | Surface treatment method for Nano diamond fine particles added to lubricant |
| CN100535070C (en) * | 2007-05-17 | 2009-09-02 | 中国地质大学（武汉） | Diamond polishing paste in high purity, and preparation method |
| WO2011011714A1 (en) * | 2009-07-23 | 2011-01-27 | International Technology Center | Lubricant additive |
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