The surface treatment method of the nano-diamond particles that in lubricating oil, adds
Technical field the present invention relates to general physical or chemical process, particularly relates to the treatment process of diamond surface being carried out the oleophylic modification.
The background technology nano-diamond particles is with detonation synthetic behind the high explosive mixing moulding.During explosive detonation, unoxidized uncombined carbon more than needed crystalline substance in the superhigh-pressure high-temp environment in detonation district becomes nano-diamond particles under the condition of negative oxygen balance.This nano-diamond particles has maximum hardness, high thermal conductivity, higher wear resistance and good adamantine general characteristics such as chemical stability, thereby, in recent years, nano-diamond particles has been attempted field widespread uses such as the grinding and polishing at chip, iron oxygen magnetic head and optical lens, compound plating, lubricated, high-intensity resin and rubber.
But nano-diamond particles also has bigger specific surface area (280~420m
2/ g) and higher surface activity.Nano diamond is owing to particle minimum (4~15 nanometer), and surface energy is high, has intensive from the tendency of reuniting, and as it not being carried out surface treatment, will directly influence its application.So when nano-diamond particles is used, at first need it is dispersed in the liquid medium.The suspension of nano-diamond particles is good more, and effect is just good more.In the prior art, never solve the surface treatment problem of nano-diamond particles well.Reunion-dispersion-suspension the problem of separating that how to solve the Nano diamond material has become the global problem of Nano diamond material application.
Application for a patent for invention 02139764 discloses separating of Nano diamond on September 3rd, 2003 reunites and stage division, and this method is a kind of hydrophilic surface modification method; In addition, this method adopts comminution by gas stream, high pressure liquid stream to pulverize or ball milling is separated reunion, and it is abundant inadequately to separate reunion, and Nano diamond particle maximum particle size reaches 200nm, the Nano diamond granule interior surface of volume particle size can not contact with chemical modifier, directly influences the Nano diamond surface modification effect; And, the hardest material of the such nature of diamond is carried out ball milling, not only there is not effect, can grind into material to milling material on the contrary, influence quality product greatly.Application for a patent for invention 02115230 discloses a kind of nano diamond particle surface treatment method on November 20th, 2002, this method is a kind of hydrophilic surface modification method equally, ultrasonic dispersing is only passed through in the reunion of separating of Nano diamond particle, it is abundant inadequately to separate reunion, causes the Nano diamond surface modification insufficient.
The summary of the invention the technical problem to be solved in the present invention is to avoid above-mentioned the deficiencies in the prior art part and the surface treatment method that proposes a kind of nano-diamond particles that adds in lubricating oil.This method combines by physical method and chemical surface modifying method, fully untie the reunion of nano-diamond particles, make Nano diamond fine particles surface coat the anchoring group of going up polymer molecule, its solvent chain fully stretches formation hyte layer in the medium again, nano-diamond particles is repelled mutually, thereby greatly improve the dispersion suspension ability of Nano diamond in lubricating oil.
The present invention solve the technical problem can be by realizing by the following technical solutions:
Propose a kind of surface treatment method of the nano-diamond particles that in lubricating oil, adds, may further comprise the steps successively,
1. usefulness high velocity air collider with Nano diamond powder head-on collision superfine grinding, is untied reunion with high velocity air;
2. the nano-diamond particles that will untie reunion is added in the organic solvent of surface-modifying agent and dispersion agent, stirring reaction is 4~12 hours under the temperature of 60~100 degree Celsius, described surface-modifying agent is a metatitanic acid fat, and dispersion agent is sodium lauryl sulphate or stearic acid;
3. utilize high-speed shearing machine to have the organic solvent high speed of nano-diamond particles to shear, and to utilize ultrasonic wave to make the microbubble internal explosion in the organic solvent be ultrasonic cavitation, thereby make nano-diamond particles further untie reunion in above-mentioned adding;
4. centrifugation goes out the nano-diamond particles after the surface modification, with organic solvent described nano-diamond particles washing back centrifugation is gone out nano-diamond particles, and dry in the environment of 50~120 degree Celsius, obtain the nano-diamond particles after the surface modification.
The present invention is by combining physics, chemical method, with the head-on collision of nano-diamond powder process high velocity air, high speed shear and ultrasonic cavitation, untie its reunion, the nano-diamond particles granularity is reduced greatly, size range is at 20~60nm, by selecting different types of surface-modifying agent, dispersion agent and solvent for use, controlling reaction time and temperature of reaction make the surface modification of nano-diamond particles very abundant then.
Embodiment is described in further detail below in conjunction with the most preferred embodiment shown in the accompanying drawing.
A kind of surface treatment method of the nano-diamond particles that adds in lubricating oil may further comprise the steps successively,
1. with the high velocity air collider with gas velocity be the high velocity air of 300~800 meter per seconds with Nano diamond powder head-on collision superfine grinding, untie reunion;
2. the nano-diamond particles that will untie reunion is added in organic solvent ethanol, toluene or the acetone of surface-modifying agent and dispersion agent, stirring reaction is 4~12 hours under the temperature of 60~100 degree Celsius, and described nano-diamond particles with the by weight/volume that is mixed with the organic solvent of surface-modifying agent and dispersion agent is: 1: 5~1: 50; Described surface-modifying agent is a metatitanic acid fat, and the weight ratio of itself and nano-diamond particles is 1~10%; Dispersion agent is sodium lauryl sulphate or stearic acid, with the weight ratio of nano-diamond particles be 1~10%;
3. utilize high-speed shearing machine to have the organic solvent high speed of nano-diamond particles to shear in above-mentioned adding with velocity of shear more than or equal to 15 meter per seconds, and utilize frequency be 28~40 kilo hertzs ultrasonic wave to make the microbubble internal explosion in the organic solvent be ultrasonic cavitation, thereby make nano-diamond particles further untie reunion;
4. centrifugation goes out the nano-diamond particles after the surface modification, with organic solvent ethanol, toluene or acetone described nano-diamond particles washing back centrifugation is gone out nano-diamond particles, look different situations, can be with nano-diamond particles repeatedly with also centrifugation behind the organic solvent washing; At last, the nano-diamond particles that will cross with organic solvent washing is dry in the baking ovens of 50~120 degree Celsius, obtains the nano-diamond particles after the surface modification.