CN108907182B - Water-soluble Cu @ SiO2 nano particle and preparation method and application thereof - Google Patents
Water-soluble Cu @ SiO2 nano particle and preparation method and application thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/10—Compounds containing silicon
- C10M2201/105—Silica
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/06—Oiliness; Film-strength; Anti-wear; Resistance to extreme pressure
Abstract
The invention belongs to the field of water-based lubricating additives, and particularly relates to water-soluble Cu @ SiO2The nano-particles are mainly prepared from the following raw materials in parts by weight: 0.1-2 parts of surface modified oil-soluble nano copper (DDP-Cu), 60-90 parts of cyclohexane, 5-15 parts of Igepal CO-5205, 0.5-7 parts of TEOS, 0.1-3 parts of ammonia water and 0.2-5 parts of distilled water. The invention also provides the water-soluble Cu @ SiO2Preparation method of nano-particles and prepared Cu @ SiO2The nano particles show excellent dispersion stability and oxidation resistance stability, show good antifriction and wear resistance when being used as a water-based lubricating additive, and have excellent application prospect.
Description
Technical Field
The invention belongs to the field of water-based lubricating additives, and particularly relates to water-soluble Cu @ SiO2A method for preparing nanoparticles and their use as water-based lubricant additives.
Background
The copper nanoparticles have low shearing force, low melting point and good self-repairing function, are widely applied to the field of tribology, and show excellent antifriction and antiwear performances. The copper nanoparticles themselves are in a chemically unstable state, and when copper nanoparticles having a small size are synthesized, agglomeration and oxidation phenomena occur due to high surface energy. To overcome this drawback, many researchers have surface-modified copper nanoparticles using surface modification techniques in order to effectively improve dispersion stability and oxidation resistance stability of the copper nanoparticles in the lubricant. It was found that the synthesis of oil-soluble copper nanoparticles is more advantageous than the synthesis of water-soluble copper nanoparticles in synthesizing high-quality copper nanoparticles.
We have previously obtained oil-soluble surface-modified oil-soluble nanocopper (hereinafter referred to as DDP-Cu nanoparticles, ZL200910065056.4, a method for preparing surface-modified oil-soluble nanocopper) having excellent tribological properties, however, since the surface modifier DDP is hydrophobic, DDP-Cu nanoparticles cannot be directly used in water-based lubrication systems. Silica itself has good tribological properties and can inhibit oxidation and agglomeration of copper nanoparticles, and the presence of a large amount of Si — OH (polar groups) on the surface of the silica shell layer contributes to a significant increase in the dispersion stability of nanoparticles in water-based lubricants.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides water-soluble Cu @ SiO2The nano-particles successfully transfer the oil-soluble DDP-Cu nano-particles into a water phase by using a silicon dioxide coating method to prepare the water-soluble Cu @ SiO with good appearance and uniform size2The nano particles have good dispersion stability and oxidation resistance stability in distilled water. The invention relates to water-soluble Cu @ SiO2The nano particles are used as a water-based lubricating additive, can effectively improve the tribological performance of distilled water, and has wide application prospect.
The invention also provides the water-soluble Cu @ SiO2A method for the preparation of nanoparticles and their use as water-based lubricant additives.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention successfully transfers the oil-soluble DDP-Cu nano particles into the water phase by using the silicon dioxide shell to coat the oil-soluble DDP-Cu nano particles to prepare the water-soluble Cu @ SiO2A nanoparticle; the water-soluble Cu @ SiO2The nano particles are mainly prepared from the following raw materials in parts by weight:
0.1-2 parts of surface-modified oil-soluble nano copper,
60-90 parts of cyclohexane,
igepal CO-5205-15 parts,
0.5 to 7 parts of TEOS (tetraethyl orthosilicate),
0.1 to 3 parts of ammonia water,
0.2-5 parts of distilled water.
The water-soluble Cu @ SiO2The preparation method of the nano-particles specifically comprises the following steps:
1) taking the raw materials according to a certain proportion, and uniformly mixing the surface modified oil-soluble nano-copper with cyclohexane to obtain a mixed solution a;
2) adding a surfactant Igepal CO-520 into the mixed solution a obtained in the step 1), and stirring to react to obtain a mixed solution b;
3) adding TEOS into the mixed solution b obtained in the step 2), and stirring for reaction to obtain a mixed solution c;
4) adding ammonia water and distilled water into the mixed solution c obtained in the step 3), and stirring and reacting for 12-40 h; after the reaction is finished, the product is obtained after centrifugal separation, washing and drying.
Specifically, in the step 1), the uniform mixing is carried out at room temperature by mixing and stirring for 5-30 min.
Specifically, in the steps 2) and 3), stirring reaction is carried out at room temperature, and the stirring reaction time is 5-30 min.
In the present invention, the raw material surface modified oil-soluble nano-copper (DDP-Cu nanoparticles) can be prepared according to patent "ZL 200910065056.4, a method for preparing surface modified oil-soluble nano-copper". The raw material surfactants Igepal CO-520 and TEOS can be purchased from common commercial products. The raw material ammonia water is strong ammonia water with the concentration of 25-28%, and common commercial products can be purchased.
The invention also provides the water-soluble Cu @ SiO2Use of nanoparticles as water-based lubricant additives.
The invention adopts a reverse microemulsion methodThe oil-soluble DDP-Cu nano particles are transferred into a water phase by coating a silicon dioxide shell layer, so that the water-soluble Cu @ SiO with uniform size and good appearance is obtained2A nanoparticle; the water-based lubricating additive is used as a water-based lubricating additive, has good dispersion stability and oxidation resistance stability, can obviously improve the antifriction and wear resistance of distilled water, and has wide application prospect. Compared with the prior art, the invention has the following advantages:
1) the invention can utilize the advantages that the oil-soluble DDP-Cu nano-particles have small particle size, uniform size and good antifriction and antiwear performance;
2) according to the invention, the oil-soluble DDP-Cu nanoparticles are transferred into the water phase by coating the silicon dioxide shell layer, the silicon dioxide shell layer has good antifriction and wear-resistant properties, and a large amount of Si-OH (polar groups) exist on the surface of the silicon dioxide shell layer, so that the dispersion stability of the nanoparticles in the water-based lubricant is remarkably improved;
3) the invention utilizes the silicon dioxide shell to coat and transfer the oil-soluble DDP-Cu nano particles into the water phase, and the silicon dioxide shell can effectively prevent the oxidation of the copper nano particles, so that the prepared water-soluble Cu @ SiO2The nanoparticles have excellent antioxidant stability;
4) the oil-soluble DDP-Cu nano-particles used in the invention can be produced in a large scale, and the preparation process equipment adopted in the invention is simple, and the raw materials are cheap and easy to obtain, so that the water-soluble Cu @ SiO nano-particles are expected to be prepared in a large scale2And (3) nanoparticles.
Drawings
FIG. 1 is a TEM photograph of oil-soluble DDP-Cu nanoparticles used in the preparation of example 1 of the present invention;
FIG. 2 shows the water-soluble Cu @ SiO prepared in example 1 of the present invention2Transmission electron micrographs of nanoparticles;
FIG. 3 shows the water-soluble Cu @ SiO prepared in example 1 of the present invention2Optical photographs of nanoparticles dispersed in distilled water;
FIG. 4 shows the water-soluble Cu @ SiO prepared in example 1 of the present invention2The nanoparticles were tested by a tribology tester to obtain tribology experimental results.
Detailed Description
The present invention will now be described in detail with reference to specific examples, which are intended to be illustrative only and should not be construed as limiting the scope of the invention. The insubstantial modifications and adaptations of the present invention as described above will now occur to those skilled in the art and are considered to be within the scope of the present invention.
In the following examples, the raw materials were used in parts by weight.
Example 1
Water-soluble Cu @ SiO2The nano particles are prepared from the following raw materials in parts by weight: 0.1 part of DDP-Cu nano-particles, 60 parts of cyclohexane, Igepal CO-5205 parts, 0.5 part of TEOS, 0.1 part of ammonia water and 0.2 part of distilled water
The water-soluble Cu @ SiO2The preparation method of the nano-particles specifically comprises the following steps:
1) adding 0.1 part of oil-soluble DDP-Cu nanoparticles into 60 parts of cyclohexane to form a mixed solution, transferring the mixed solution into a three-neck flask, and stirring for 20min under an inert gas atmosphere (the three-neck flask is subjected to exhaust treatment by inert gas in advance to remove oxygen) to uniformly mix to obtain a mixed solution a;
2) adding 5 parts of surfactant Igepal CO-520 into the mixed solution a obtained in the step 1), and stirring and reacting for 20min at room temperature to obtain a mixed solution b;
3) adding 0.5 part of TEOS into the mixed solution b obtained in the step 2), and stirring and reacting for 20min at room temperature to obtain a mixed solution c;
4) adding 0.1 part of ammonia water and 0.2 part of distilled water into the mixed solution c obtained in the step 3), and stirring and reacting for 12 hours; after the reaction is finished, centrifugally separating, washing and drying to obtain the catalyst.
FIG. 1 is a TEM photograph of oil-soluble DDP-Cu nanoparticles used in the preparation of example 1; FIG. 2 shows the water-soluble Cu @ SiO prepared in example 12Transmission electron micrograph of nanoparticles. It can be seen from FIG. 1 that: the oil-soluble DDP-Cu nanoparticles have small particle size, are dispersed very uniformly and have an average particle size of about 4 nm. As can be seen from fig. 2: preparing the obtained water-soluble Cu @ SiO2The nano particles are in good spherical shape, uniform in particle size and good in dispersity. The oil-soluble DDP-Cu nanoparticles are well coated in the silicon dioxide spheres, and the aggregation phenomenon cannot occur in the silicon dioxide spheres.
Example 2
Water-soluble Cu @ SiO2The nano-particles are prepared from the following raw materials in parts by weight: 0.5 part of DDP-Cu nano-particles, 65 parts of cyclohexane, Igepal CO-5207 parts, 1 part of TEOS, 0.3 part of ammonia water and 0.9 part of distilled water
The water-soluble Cu @ SiO2The preparation method of the nano-particles specifically comprises the following steps:
1) adding 0.5 part of oil-soluble DDP-Cu nanoparticles into 65 parts of cyclohexane to form a mixed solution, transferring the mixed solution into a three-neck flask, and stirring for 10min under an inert gas atmosphere (the three-neck flask is subjected to exhaust treatment by inert gas in advance to remove oxygen) to uniformly mix to obtain a mixed solution a;
2) adding 7 parts of surfactant Igepal CO-520 into the mixed solution a obtained in the step 1), and stirring and reacting for 10min at room temperature to obtain a mixed solution b;
3) adding 1 part of TEOS into the mixed solution b obtained in the step 2), and stirring and reacting for 10min at room temperature to obtain a mixed solution c;
4) adding 0.3 part of ammonia water and 0.9 part of distilled water into the mixed solution c obtained in the step 3), and stirring for reacting for 17 hours; after the reaction is finished, centrifugally separating, washing and drying to obtain the catalyst.
Example 3
Water-soluble Cu @ SiO2The nano-particles are prepared from the following raw materials in parts by weight: 0.8 part of DDP-Cu nano-particles, 72 parts of cyclohexane, Igepal CO-5209 parts, 1.5 parts of TEOS, 0.9 part of ammonia water and 1.7 parts of distilled water
The water-soluble Cu @ SiO2The preparation method of the nano-particles specifically comprises the following steps:
1) adding 0.8 part of oil-soluble DDP-Cu nanoparticles into 72 parts of cyclohexane to form a mixed solution, transferring the mixed solution into a three-neck flask, and stirring for 20min under an inert gas atmosphere (the three-neck flask is subjected to exhaust treatment by inert gas in advance to remove oxygen) to uniformly mix to obtain a mixed solution a;
2) adding 9 parts of surfactant Igepal CO-520 into the mixed solution a obtained in the step 1), and stirring and reacting for 20min at room temperature to obtain a mixed solution b;
3) adding 1.5 parts of TEOS into the mixed solution b obtained in the step 2), and stirring and reacting for 20min at room temperature to obtain a mixed solution c;
4) adding 0.9 part of ammonia water and 1.7 parts of distilled water into the mixed solution c obtained in the step 3), and stirring and reacting for 26 hours; after the reaction is finished, centrifugally separating, washing and drying to obtain the catalyst.
Example 4
Water-soluble Cu @ SiO2The nano-particles are prepared from the following raw materials in parts by weight: 1 part of DDP-Cu nano-particles, 83 parts of cyclohexane, Igepal CO-52010 parts, 5 parts of TEOS, 1.9 parts of ammonia water and 2.5 parts of distilled water
The water-soluble Cu @ SiO2The preparation method of the nano-particles specifically comprises the following steps:
1) adding 1 part of oil-soluble DDP-Cu nanoparticles into 83 parts of cyclohexane to form a mixed solution, transferring the mixed solution into a three-neck flask, and stirring for 30min under an inert gas atmosphere (the three-neck flask is subjected to exhaust treatment by inert gas in advance to remove oxygen) to uniformly mix to obtain a mixed solution a;
2) adding 10 parts of surfactant Igepal CO-520 into the mixed solution a obtained in the step 1), and stirring and reacting for 30min at room temperature to obtain a mixed solution b;
3) adding 5 parts of TEOS into the mixed solution b obtained in the step 2), and stirring and reacting for 30min at room temperature to obtain a mixed solution c;
4) adding 1.9 parts of ammonia water and 2.5 parts of distilled water into the mixed solution c obtained in the step 3), and stirring for reacting for 32 hours; after the reaction is finished, centrifugally separating, washing and drying to obtain the catalyst.
Example 5
Water-soluble Cu @ SiO2Nanoparticles consisting ofThe raw materials are prepared as follows: 1.5 parts of DDP-Cu nano particles, 89 parts of cyclohexane, Igepal CO-52012 parts, 6 parts of TEOS, 2.3 parts of ammonia water and 3.9 parts of distilled water
The water-soluble Cu @ SiO2The preparation method of the nano-particles specifically comprises the following steps:
1) adding 1.5 parts of oil-soluble DDP-Cu nanoparticles into 89 parts of cyclohexane to form a mixed solution, transferring the mixed solution into a three-neck flask, and stirring for 30min under an inert gas atmosphere (the three-neck flask is subjected to exhaust treatment by inert gas in advance to remove oxygen) to uniformly mix to obtain a mixed solution a;
2) adding 12 parts of surfactant Igepal CO-520 into the mixed solution a obtained in the step 1), and stirring and reacting for 30min at room temperature to obtain a mixed solution b;
3) adding 6 parts of TEOS into the mixed solution b obtained in the step 2), and stirring and reacting for 30min at room temperature to obtain a mixed solution c;
4) adding 2.3 parts of ammonia water and 3.9 parts of distilled water into the mixed solution c obtained in the step 3), and stirring for reacting for 38 hours; after the reaction is finished, centrifugally separating, washing and drying to obtain the catalyst.
Application test:
FIG. 3 shows the water-soluble Cu @ SiO prepared in example 1 of the present invention2Optical photographs (left for 1 month) of nanoparticles dispersed in distilled water (right panel) and oil-soluble DDP-Cu nanoparticles dispersed in cyclohexane (left panel), as seen in fig. 3: the oil-soluble DDP-Cu nanoparticles are completely transferred into a water phase after being coated by silicon dioxide, and can stably exist in a water phase medium.
FIG. 4 shows the water-soluble Cu @ SiO prepared in example 1 of the present invention2Results of tribological Performance testing of nanoparticles as water-based lubricating additives (Instrument model UMT-2, CETR Corp., USA, amplitude: 5 mm; frequency: 2 Hz; load: 4N; test time: 30 min).
As can be seen from the a diagram in fig. 4: the coefficient of friction of pure distilled water is 0.3902; 0.2 wt.% of Cu @ SiO prepared as in example 1 was added2After the nanoparticles are adopted, the friction coefficient is reduced from 0.3902 to 0.2103, and is reduced by 46.10%; 0.4wt% of the product of example 1 was addedPreparing the obtained Cu @ SiO2After the nanoparticles are added, the friction coefficient is reduced from 0.3902 to 0.171, which is reduced by 56.18%; 0.6 wt.% of Cu @ SiO prepared as in example 1 was added2After the nanoparticles are added, the friction coefficient is reduced from 0.3902 to 0.1965, which is reduced by 49.64%; 0.8 wt.% of Cu @ SiO, prepared as in example 1, was added2After the nanoparticles are adopted, the friction coefficient is reduced from 0.3902 to 0.2265, and is reduced by 41.95%; 1.0 wt.% of Cu @ SiO prepared as in example 1 was added2After the nanoparticles are adopted, the friction coefficient is reduced from 0.3902 to 0.3052, and the reduction is 21.78%; through comparison, the Cu @ SiO prepared by the invention2The nano-particles have good antifriction performance.
As can be seen from graph b in FIG. 4, the abrasion volume of the pure distilled water is 1.05 × 10-4mm3N · m; 0.2 wt.% of Cu @ SiO prepared as in example 1 was added2After nanoparticles, the attrition volume was from 1.05 × 10-4mm3The value of/N.m is reduced to 6.24 × 10-6mm3The concentration of/N.m is reduced by 94.06%; 0.4% by weight of Cu @ SiO as prepared in example 1 was added2After nanoparticles, the attrition volume was from 1.05 × 10-4mm3The value of/N.m is reduced to 6.87 × 10-6mm3The concentration of/N.m is reduced by 93.46%; 0.6 wt.% of Cu @ SiO prepared as in example 1 was added2After nanoparticles, the attrition volume was from 1.05 × 10-4mm3The value of/N.m is reduced to 7.27 × 10-6mm3The concentration of/N.m is reduced by 93.08%; 0.8 wt.% of Cu @ SiO, prepared as in example 1, was added2After nanoparticles, the attrition volume was from 1.05 × 10-4mm3The value of/N.m is reduced to 1.17 × 10-5mm3The concentration of/N.m is reduced by 88.86%; 1.0 wt.% of Cu @ SiO prepared as in example 1 was added2After nanoparticles, the attrition volume was from 1.05 × 10-4mm3The value of/N.m is reduced to 1.91 × 10-5The reduction is 81.81%; through comparison, the Cu @ SiO prepared by the invention2The nano-particles have good abrasion resistance.
Water-soluble Cu @ SiO prepared in examples 2 to 52The nanoparticles were also tribologically tested. The experimental results show that: properties of the products obtained in examples 2 to 5 and examples1 water-soluble Cu @ SiO2The nano particles have equivalent antifriction and wear resistance, namely, the friction coefficient can be effectively reduced, the wear volume can be reduced, the tribological performance of distilled water can be improved, and the nano particles have better application prospect.
In summary, it can be seen that: the oil-soluble DDP-Cu nanoparticles are successfully transferred into a water phase medium by coating a silicon dioxide shell layer; prepared water-soluble Cu @ SiO2The nano particles have good appearance, uniform size and good dispersion stability, and can effectively improve the antifriction and antiwear performance of distilled water when being used as a water-based lubricating additive. The invention provides a new idea for preparing water-soluble nano particles and has a very good development prospect.
Claims (4)
1. Water-soluble Cu @ SiO2Use of nanoparticles as water-based lubricant additives, characterized in that the water-soluble Cu @ SiO2The nano particles are mainly prepared from the following raw materials in parts by weight:
0.1-2 parts of surface-modified oil-soluble nano copper,
60-90 parts of cyclohexane,
igepal CO-5205-15 parts,
0.5 to 7 parts of TEOS,
0.1 to 3 parts of ammonia water,
0.2-5 parts of distilled water.
2. The water soluble Cu @ SiO of claim 12The preparation method of the nano-particles is characterized by comprising the following steps:
1) taking the raw materials according to a certain proportion, and uniformly mixing the surface modified oil-soluble nano copper with cyclohexane in an inert gas atmosphere to obtain a mixed solution a;
2) adding Igepal CO-520 into the mixed solution a obtained in the step 1), and stirring to react to obtain a mixed solution b;
3) adding TEOS into the mixed solution b obtained in the step 2), and stirring for reaction to obtain a mixed solution c;
4) adding ammonia water and distilled water into the mixed solution c obtained in the step 3), and stirring and reacting for 12-40 h; after the reaction is finished, the product is obtained after centrifugal separation, washing and drying.
3. The water soluble Cu @ SiO of claim 22The preparation method of the nano-particles is characterized in that in the step 1), the uniform mixing is carried out at room temperature through mixing and stirring, and the mixing and stirring time is 5-30 min.
4. The water soluble Cu @ SiO of claim 22The preparation method of the nano-particles is characterized in that in the steps 2) and 3), stirring reaction is carried out at room temperature, and the stirring reaction time is 5-30 min.
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Effective date of registration: 20221025 Address after: No.192 Longshoushan Road, Huangdao District, Qingdao City, Shandong Province 266000 Patentee after: QINGDAO COPTON PETROCHEMICAL CO.,LTD. Address before: 475001 Henan province city Minglun Street No. 85 Patentee before: Henan University |