CN110357090B - Preparation method of nano-diamond hydrosol - Google Patents
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Abstract
The invention discloses a preparation method of a nano-diamond hydrosol. The preparation method of the nano-diamond hydrosol comprises the following steps: 1) placing the nano-diamond raw powder in an electromagnetic field for treatment to obtain surface-modified nano-diamond powder; 2) mixing the surface modified nano-diamond powder with water, and carrying out ultrasonic treatment to obtain the nano-diamond hydrosol. The preparation method of the nano-diamond hydrosol provided by the invention is beneficial to solving the problems of easy agglomeration, difficult long-term stability and complicated process operation of nano-diamond dispersion in water, reduces the process steps while ensuring excellent dispersion and improves the preparation efficiency.
Description
Technical Field
The invention belongs to the technical field of nano-diamond processing, and particularly relates to a preparation method of a nano-diamond hydrosol.
Background
The nano-diamond has the composite characteristics of nano-materials and superhard materials, is widely applied to the fields of biomedicine, petrochemical industry, material polishing, composite plating and the like due to the excellent performance, and has extremely wide application prospect.
Nanodiamond applications are primarily limited by their degree of dispersion. The inherent size effect, surface effect and close range effect of the nano powder exacerbate the complexity of the dispersion process. The single particle size of the nano diamond with the purity of 70-97 percent is only 60nm at the thickest, the average particle size is 10-12 nm, however, the average particle size of the purchased commercial diamond is more than 2 μm, and the thickest diamond can reach 10 μm, and the nano diamond is accompanied with large agglomeration. The reason why the agglomerates exist in the nano diamond powder may be that carbon particles formed at ultra-high temperature and high pressure during detonation are mutually condensed in a cooling process to form hard agglomerates with large particle size, and that the particles of a dehydration product after detonation are close to each other due to capillary suction in a nano powder drying process to form hard agglomerates.
In order to solve the primary problem that the application of the nano-diamond hydrosol is influenced by hard agglomeration of nano-diamond, in the prior art, the surface groups of the nano-diamond are modified by a chemical method or a mechanical treatment method, and the nano-diamond is dispersed in water by changing the hydrophilic or hydrophobic characteristics of the surface groups of nano-diamond particles under the synergistic action of a chemical reagent and physical vibration. CN104261404A discloses a preparation method of super-dispersed nano diamond hydrosol, which comprises the following main components: nano-diamond, concentrated acid, deionized water and corresponding ball milling beads; the main method comprises the steps of firstly carrying out acidizing treatment on the nano-diamond raw powder, adding a certain amount of ball milling beads and deionized water, mixing, carrying out wet ball milling, finally carrying out ultrasonic dispersion on the obtained nano-diamond suspension and the ball milling beads, and carrying out centrifugation to remove impurities. Although the technical scheme obtains the nano-diamond suspension with smaller particle size, impurities which are difficult to remove can be introduced by adding the ball milling beads, and the requirements on the proportion of raw materials and concentrated acid and the temperature of reaction kettle equipment are high. For another example, CN1380363A discloses a method for surface treatment of nanodiamond, in which nanodiamond is dispersed in an organic solvent of a silane surface modification reagent, and the specific process steps are as follows: the nano-diamond particles with different active groups on the surface can be obtained by ultrasonically dispersing the nano-diamond in a common anhydrous organic solvent containing a silane surface modification reagent, carrying out stirring reaction for 24-48 hours, then centrifugally separating the nano-diamond particles, using the common anhydrous organic solvent once, and carrying out vacuum drying at a constant temperature of 50-60 ℃ for 24-48 hours. Although the technical scheme realizes the preparation of the nano-diamond sol, the problems are obvious, the selection of the anhydrous organic solvent and the solid-liquid ratio are difficult to control, the whole operation steps are complex, and the use of chemical reagents is more complicated.
The existing preparation technology of the nano-diamond hydrosol has the following defects or shortcomings: firstly, because the size and the distribution of particles can be controlled by ultrasonic dispersion, and the obtained product is distributed more uniformly, the ultrasonic dispersion technology is often used in chemical production, but the single ultrasonic dispersion can not ensure the long-term stability of hydrosol, and has higher requirements on ultrasonic temperature and power. Secondly, because the nano-diamond is often agglomerated into a massive aggregate, the prior art mostly adopts mechanical grinding or auxiliary ball milling to refine the diamond powder. However, mechanical or ball milling processing often cannot avoid introducing larger impurities, so that the purity of the nano-diamond hydrosol is reduced, the later impurity removal cost is increased, and the application of the nano-diamond hydrosol is greatly influenced. In order to change the hydrophilicity and hydrophobicity of the surface groups of the nano-diamond, the prior art also comprises a chemical dispersion technical method, chemical linkage is generated through a reactive organic compound, and the nano-particles are soluble in an organic medium due to the organic compound branched chains or groups connected to the surfaces of the nano-particles, so that the dispersion of the nano-particles in the organic medium is enhanced. But the environmental requirements on chemical reaction are very high, and the selection and solid-liquid ratio of organic media are also very limited. In the current research technology, dispersing agents are also commonly used for dispersing. The dispersing agent is a surfactant which can obviously change the surface or interface properties of a substance by a small amount, the dispersing effect is achieved by changing the surface charge of the nano particles, and after the dispersing agent is added, other chemical substances are mixed in the aqueous solution or the organic solvent, so that the application of the nano diamond in the fields of biological medicine and the like is hindered. And fifthly, the stability of the nano-diamond hydrosol is seriously influenced due to various reasons that the nano-diamond is not stable in thermodynamics and has high specific surface energy and the like. Therefore, the composite dispersion method is one of the important development trends for realizing the preparation of the nano-diamond hydrosol, but is limited by the complexity of each process and the requirement on the environment, and the processes are difficult to be well combined in the field of the preparation of the nano-diamond hydrosol, so that the nano-diamond hydrosol which is suitable for large-scale industrial production and has simple and convenient process is obtained.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a method for preparing a nano-diamond hydrosol, which aims to solve the problems of easy agglomeration, difficult long-term stabilization and complex process existing in the dispersion of nano-diamond in water.
The technical scheme adopted by the invention is as follows:
the invention provides a preparation method of a nano-diamond hydrosol. The preparation method of the nano-diamond hydrosol comprises the following steps:
1) placing the nano-diamond raw powder in an electromagnetic field for treatment to obtain surface-modified nano-diamond powder;
2) mixing the surface modified nano-diamond powder with water, and carrying out ultrasonic treatment to obtain the nano-diamond hydrosol.
Preferably, in step 1) of the method for preparing the nano-diamond hydrosol, the frequency range of the electromagnetic field is 2 × 109Hz～2×1020Hz; further preferably, the frequency range of the electromagnetic field is 1 × 1010Hz～2×1019Hz。
Preferably, in step 1) of the method for preparing a nanodiamond hydrosol, the electromagnetic wave of the electromagnetic field may be selected from the group consisting of radio wave, X-ray, infrared ray or ultraviolet ray. The radio waves include microwaves.
Preferably, in the step 1) of the preparation method of the nano-diamond hydrosol, the treatment is carried out under the heating condition, and the heating temperature is 50-700 ℃; further preferably, the heating temperature is 100 ℃ to 680 ℃; still more preferably, the heating temperature is 120 to 650 ℃.
Preferably, in the step 1) of the preparation method of the nano-diamond hydrosol, the treatment is carried out under a certain pressure intensity, and the treatment pressure intensity is 1 kPa-1 MPa; further preferably, the pressure of the treatment is 1kPa to 20 kPa; still further preferably, the pressure of the treatment is 1 to 10 kPa; more preferably, the pressure of the treatment is 1kPa to 5 kPa.
Preferably, in the step 1) of the preparation method of the nano-diamond hydrosol, the treatment time is 1-30 min; further preferably, the treatment time is 3min to 25 min; still more preferably, the treatment time is 5 to 20 min.
Preferably, in step 1) of the method for preparing the nano-diamond hydrosol, the particle size of the nano-diamond raw powder (the size of a single nano-diamond particle) is 8nm to 12 nm; the purity (mass content of the nano-diamond) of the nano-diamond raw powder is more than or equal to 94 percent.
Preferably, in step 1) of the method for preparing the nano-diamond hydrosol, the nano-diamond raw powder is nano-diamond obtained by a detonation methodStone raw powder. The nano-diamond particles prepared by the method are sp3The polyhedron formed by diamond cores made of carbon has a large number of dangling bonds connected with functional groups, has unsaturation, is easy to combine with other atoms, and contains nitrogen and hydrogen impurities (up to 2-3 wt%). The nano diamond raw powder is easy to agglomerate in a solvent system in practical application, and the average particle size after agglomeration reaches hundreds of nanometers and even more than 1 micron.
In the preparation method of the nano-diamond hydrosol, step 1), the surface modified nano-diamond powder refers to surface hydrophilic modified nano-diamond powder.
Preferably, in step 2) of the method for preparing the nano-diamond hydrosol, the mixing ratio of the surface-modified nano-diamond powder to water is 1 g: (5-20) mL; further preferably, the mixing ratio of the surface-modified nano diamond powder to water is 1 g: (8-12) mL.
Preferably, in step 2) of the method for preparing the nano-diamond hydrosol, the water is deionized water.
Preferably, in the step 2) of the preparation method of the nano-diamond hydrosol, the ultrasonic frequency of ultrasonic treatment is 18 kHz-25 kHz; further preferably, the ultrasonic frequency of the ultrasonic treatment is 20 kHz.
Preferably, in the step 2) of the preparation method of the nano-diamond hydrosol, the power of ultrasonic treatment is 100W-1000W; further preferably, the power of ultrasonic treatment is 200W-900W; still more preferably, the power of the ultrasonic treatment is 300W to 800W.
Preferably, in the step 2) of the preparation method of the nano-diamond hydrosol, the ultrasonic treatment time is 30-100 min; further preferably, the time of the ultrasonic treatment is 50 to 70 min.
Preferably, in step 2) of the method for preparing the nano-diamond hydrosol, cooling water is introduced for cooling during ultrasonic treatment.
The invention also provides the nano-diamond hydrosol prepared by the preparation method.
The invention has the beneficial effects that:
the preparation method of the nano-diamond hydrosol provided by the invention is beneficial to solving the problems of easy agglomeration, difficult long-term stability and complicated process operation of nano-diamond dispersion in water, reduces the process steps while ensuring excellent dispersion and improves the preparation efficiency.
Compared with the prior art, the invention has the following specific advantages:
1) the method has the advantages of simple technical process, easy large-scale production, high production efficiency and easy operation and execution, and the treated nano-diamond can be uniformly and stably dispersed in water to form stable colloidal solution.
2) The invention utilizes an electromagnetic field to modify the surface functional groups of the nano-diamond powder, thereby changing the hydrophilicity of the nano-diamond powder, not generating any adverse effect on the environment in the whole experimental process and meeting the industrial greenization.
3) The invention does not use any chemical dispersing reagent, wetting reagent and the like, is applied to the industrial fields such as the traditional precision polishing field and the like, is also suitable for the emerging fields such as biomedicine, composite plating and the like, and has great application prospect.
4) The invention does not use any ball milling and mechanical oscillation auxiliary treatment, thereby greatly reducing the foreign impurity components and reducing the impurity removal cost.
5) The invention uses less instruments and experimental raw materials and reduces the production cost.
Drawings
FIG. 1 is a schematic flow diagram of a process for preparing a nanodiamond hydrosol;
FIG. 2 is an infrared spectrum of the nanodiamond raw powder and the modified nanodiamond;
fig. 3 is an XRD pattern of the nanodiamond raw powder and the modified nanodiamond;
FIG. 4 is a graph showing the distribution of the particle sizes of the nanodiamond raw powder and the modified nanodiamond;
fig. 5 is a graph of an untreated nanodiamond hydrosol;
fig. 6 is a diagram of a surface modified nanodiamond hydrosol.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials used in the examples are, unless otherwise specified, commercially available from conventional sources.
The nano-diamond raw powder obtained by the detonation method used in the following examples had a single particle size of 10nm and a purity (nano-diamond mass content) of 95 wt%. The particle sizes in the examples were measured by DLS (dynamic light scattering particle size analyzer).
Example 1
Fig. 1 is a flow chart showing a method for preparing a nano-diamond hydrosol, and ND in fig. 1 denotes nano-diamonds (Nanodiamonds). The following description, with reference to fig. 1, illustrates the preparation method of the nano-diamond hydrosol of this example including the following steps:
1) 20g of nano-diamond raw powder obtained by a detonation method is subjected to 2 multiplied by 10 frequency10Hz, 3kPa, 550 ℃ for 5min, and obtaining the surface modified nano-diamond powder.
And respectively carrying out Fourier infrared spectrum, XRD characterization and particle size analysis on the nano-diamond raw powder and the modified nano-diamond. FIG. 2 is an infrared spectrum of the nano-diamond raw powder and the modified nano-diamond. Figure 3 is an XRD pattern of the nanodiamond raw powder and the modified nanodiamond. FIG. 4 is a graph showing the distribution of the particle sizes of the nanodiamond raw powder and the modified nanodiamond. The test results of fig. 2-4 show that the modified nanodiamond has more hydrophilic functional groups on the surface and a more obvious reduction in particle size compared with the nanodiamond raw powder.
2) Taking out 2g of nano-diamond powder with the modified surface, adding 20mL of deionized water, carrying out ultrasonic treatment by using an ultrasonic machine, wherein the power is 500W, the ultrasonic treatment time is 1h, the ultrasonic frequency is 20kHz, and meanwhile, in order to prevent the ultrasonic temperature from being overhigh, cooling water with the temperature of 0 ℃ is introduced for cooling.
And after ultrasonic treatment, obtaining the nano diamond hydrosol with the final particle size of 10-100 nm. The untreated nano-diamond hydrosol is shown in figure 5, and the average particle size is 150-200 nm. The surface-modified nano-diamond hydrosol of the embodiment can be seen in figure 6, and the average particle size is 10-100 nm. The nano-diamond hydrosol obtained in the example can keep stable within 30 days, and no obvious precipitation is found.
Example 2
The preparation method of the nano-diamond hydrosol comprises the following steps:
1) 20g of nano-diamond raw powder obtained by a detonation method is added at the frequency of 1010Placing in a high-energy microwave field with Hz, pressure of 5kPa and temperature of 120 ℃ for 10min to obtain the surface modified nano-diamond powder.
2) And (3) taking out 2g of nano-diamond powder with the modified surface, adding 20mL of deionized water, carrying out ultrasonic treatment by using an ultrasonic machine, wherein the power is 400W, the ultrasonic treatment time is 1h, the ultrasonic treatment frequency is 20kHz, and meanwhile, introducing cooling water with the temperature of 0 ℃ for cooling.
And after ultrasonic treatment, obtaining the nano diamond hydrosol with the final particle size of 10-100 nm.
Example 3
The preparation method of the nano-diamond hydrosol comprises the following steps:
1) 20g of nano-diamond raw powder obtained by a detonation method is subjected to 2 multiplied by 10 frequency19Placing in an X-ray field with Hz, pressure of 5kPa and temperature of 650 ℃ for 20min to obtain the surface modified nano-diamond powder.
2) And taking out 2g of nano-diamond powder with the modified surface, adding 20mL of deionized water, carrying out ultrasonic treatment by using an ultrasonic machine, wherein the power is 600W, the ultrasonic treatment time is 1h, the ultrasonic frequency is 20kHz, and meanwhile, cooling water with the temperature of 0 ℃ is introduced for cooling.
And after ultrasonic treatment, obtaining the nano diamond hydrosol with the final particle size of 10-100 nm.
Example 4
The preparation method of the nano-diamond hydrosol comprises the following steps:
1) 20g of nano-diamond raw powder obtained by a detonation method is put at a frequency of 2 multiplied by 1012Hz, the pressure is 3kPa, the temperature is 450 ℃ for 20min, and the nano diamond powder after surface modification is obtained.
2) And (3) taking out 2g of nano-diamond powder with the modified surface, adding 20mL of deionized water, carrying out ultrasonic treatment by using an ultrasonic machine, wherein the power is 300W, the ultrasonic treatment time is 1h, the ultrasonic treatment frequency is 20kHz, and meanwhile, introducing cooling water with the temperature of 0 ℃ for cooling.
And after ultrasonic treatment, obtaining the nano diamond hydrosol with the final particle size of 10-100 nm.
Example 5
The preparation method of the nano-diamond hydrosol comprises the following steps:
1) 20g of nano-diamond raw powder obtained by a detonation method is put at a frequency of 1016Hz, the pressure is 1kPa, the temperature is 200 ℃ for 20min, and the nano diamond powder after surface modification is obtained.
2) And (3) taking out 2g of nano-diamond powder with the modified surface, adding 20mL of deionized water, carrying out ultrasonic treatment by using an ultrasonic machine, wherein the power is 800W, the ultrasonic treatment time is 1h, the ultrasonic treatment frequency is 20kHz, and meanwhile, introducing cooling water with the temperature of 0 ℃ for cooling.
And after ultrasonic treatment, obtaining the nano diamond hydrosol with the final particle size of 10-100 nm.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A method for preparing nano-diamond hydrosol is characterized by comprising the following steps: the method comprises the following steps:
1) placing the nano-diamond raw powder in an electromagnetic field for treatment to obtain surface-modified nano-diamond powder;
2) mixing the surface-modified nano-diamond powder with water, and performing ultrasonic treatment to obtain nano-diamond hydrosol;
in the step 1), the nano-diamond raw powder is obtained by a detonation method; the frequency range of the electromagnetic field is 2 x 109Hz~2×1020Hz。
2. The method of claim 1, wherein: in the step 1), the treatment is carried out under the heating condition, wherein the heating temperature is 50-700 ℃.
3. The method of claim 1, wherein: in the step 1), the treatment is carried out under a certain pressure, and the pressure of the treatment is 1 kPa-1 MPa.
4. The method of claim 1, wherein: in the step 1), the treatment time is 1-30 min.
5. The method of claim 1, wherein: in the step 2), the mixing ratio of the surface modified nano-diamond powder to water is 1 g: (5-20) mL.
6. The method of claim 1, wherein: in the step 2), the power of ultrasonic treatment is 100W-1000W, and the time of ultrasonic treatment is 30 min-100 min.
7. The nanodiamond hydrosol prepared by the preparation method according to any one of claims 1 to 6.
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