CN110124548B - Preparation method of nanoparticle water dispersion - Google Patents
Preparation method of nanoparticle water dispersion Download PDFInfo
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- CN110124548B CN110124548B CN201910320223.9A CN201910320223A CN110124548B CN 110124548 B CN110124548 B CN 110124548B CN 201910320223 A CN201910320223 A CN 201910320223A CN 110124548 B CN110124548 B CN 110124548B
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- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/50—Mixing liquids with solids
- B01F23/53—Mixing liquids with solids using driven stirrers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
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Abstract
A method of preparing an aqueous dispersion of nanoparticles comprising: mixing raw material nanoparticles and water according to a preset mass ratio, and mechanically stirring at a preset rotating speed for a first preset time to obtain nanoparticle slurry; adding the nano particle slurry into a high-pressure homogenizer for shearing so as to reduce the particle size of the nano particles in the nano particle slurry; and finally, adding the sheared nanoparticle slurry into a micro-jet homogenizer for secondary shearing to obtain a nanoparticle aqueous dispersion, wherein the particle size of the nanoparticles in the nanoparticle aqueous dispersion is 50-300 nm. The nano particle aqueous dispersion is prepared by shearing with a high-pressure homogenizer and secondary shearing with a micro-jet homogenizer, and the size of nano particles can be controlled by adjusting the pressure and the processing time of the shearing with the high-pressure homogenizer and the micro-jet homogenizer in the preparation process, so that the prepared nano particle aqueous dispersion has better stability. The method is simple, does not need to use organic solvent and stabilizer, and does not have the problems of environmental pollution and subsequent waste liquid treatment.
Description
Technical Field
The invention relates to the technical field of nanoparticles, in particular to a preparation method of a nanoparticle aqueous dispersion.
Background
The size of the nanoparticle has an important influence on the physical properties and chemical characteristics thereof, and the nanoparticle has many excellent physical properties and chemical properties such as electricity, light, magnetism, force, heat and the like due to the small size effect, the surface effect, the quantum size effect and the like. In many production processes, it is required that the nanoparticles are uniformly and stably dispersed in a liquid-phase medium, for example: paints, pharmaceuticals, dyes, and cosmetic preparations, etc.; in recent years, whether the nano-particle oil displacement agent used in the petroleum tertiary recovery can be uniformly dispersed in an aqueous medium or not and the size of the nano-particle directly influences the application effect of the nano-particle oil displacement agent on site.
However, the nanoparticles have a large specific surface area and a high surface energy, and the nanoparticles suspended in the liquid tend to agglomerate with each other to reduce the surface energy thereof, and in addition, the suspended nanoparticles undergo random brownian motion to collide with each other to form agglomerates, so that the dispersion degree of the nanoparticles is reduced, and the agglomerates settle under the action of gravity, so that the stability of the nanosuspension is reduced. Therefore, the collision frequency and the agglomeration trend among the nano particles in the nano suspension are reduced, so that the nano particles are uniformly dispersed and stably suspended in the base solution, and finally the uniformly dispersed and stably suspended nano suspension becomes a research hotspot.
According to different dispersion methods, methods for improving the stability of the nano-suspension can be divided into a physical dispersion method and a chemical dispersion method, wherein the physical dispersion method mainly comprises ultrasonic dispersion and mechanical dispersion, and the chemical dispersion method mainly comprises adding a dispersing agent, adjusting the pH value of the suspension, modifying the surface of the nano-particles and the like.
The ultrasonic dispersion method in physical methods is a method for generating cavitation action on liquid by utilizing the dispersion effect of ultrasonic waves in the liquid so as to break solid particles in the liquid and increase the stability of dispersion liquid, and the particle size of a processed product is not uniform along with larger noise in the ultrasonic treatment process; mechanical dispersion is a method of dispersing nanoparticles by means of impact force or shear force generated by mechanical equipment, and the like, and a ball milling dispersion method and a mechanical stirring dispersion method are common, and the ball milling dispersion method can crush nanoparticles, reduce the particle size and increase the stability of a dispersion liquid. However, in the ball milling and dispersing process, the ball body and the milling barrel are easy to generate abrasion substances, so that the purity of the nano material is influenced; the mechanical stirring is generally to continuously stir the nanoparticle suspension by magnetic stirring or the like to suspend the nanoparticles in the liquid, so as to achieve the effect of dispersion, and once the stirring is stopped, the nanoparticles are re-aggregated, so that the nanoparticle dispersion system cannot maintain a stable dispersion state.
A method for preparing rutile type nanometer titanium dioxide particles with controllable particle sizes comprises the steps of preparing titanium dioxide seed crystals by using perchloric acid and titanium isopropoxide, and then preparing rutile nanometer particles through hydrothermal reaction.
A method of preparing graphene, which prepares a feed solution by homogenizing expanded graphite at a high speed and then homogenizes the feed solution at a high pressure, thereby improving high-pressure homogenization efficiency by improving dispersibility of the expanded graphite in the feed solution. The method for preparing the graphene is simple and uniform in size, the method used in the invention belongs to mechanical dispersion in a physical dispersion method, the process is simpler, but in the invention, various dispersing agents are used for improving the dispersion degree of the expanded graphite and the graphene to maintain the dispersion state of the expanded graphite and the graphene, and the purity of the product is influenced.
Although a plurality of methods for preparing nanoparticle dispersion liquid are disclosed at present, part of the methods can realize particle size control, wherein a chemical method relates to the use of a plurality of organic solvents and chemical reagents, so that environmental pollution and certain potential safety hazard exist, and part of chemical modification only aims at specific nanoparticles and functional groups and has great limitation; compared with the prior art, the physical method is more environment-friendly and safer, but the physical method has the problems of low dispersion efficiency, long treatment time, high equipment energy consumption and the like, so that the method has great significance for finding a dispersion method which is efficient, environment-friendly and wide in application range on the basis of the prior art.
Disclosure of Invention
Objects of the invention
The invention aims to provide a preparation method of a nanoparticle aqueous dispersion, which is characterized in that the nanoparticle aqueous dispersion is prepared by shearing through a high-pressure homogenizer and secondary shearing through a micro-jet homogenizer, and the size of nanoparticles can be controlled by adjusting the pressure and the treatment time of the shearing through the high-pressure homogenizer and the micro-jet homogenizer in the preparation process, so that the prepared nanoparticle aqueous dispersion has good stability and can be stably placed for one month or more.
(II) technical scheme
In order to solve the above problems, according to one aspect of the present invention, there is provided a method for preparing an aqueous dispersion of nanoparticles, comprising:
s1: mixing raw material nanoparticles and water according to a preset mass ratio, and mechanically stirring at a preset rotating speed for a first preset time to obtain nanoparticle slurry;
s2: adding the nano particle slurry into a high-pressure homogenizer for shearing so as to reduce the particle size of the nano particles in the nano particle slurry;
s3: and adding the sheared nanoparticle slurry into a micro-jet homogenizer for secondary shearing to obtain a nanoparticle aqueous dispersion, wherein the particle size of the nanoparticles in the nanoparticle aqueous dispersion is 50-300 nm.
Further, step S2 is performed 3-6 times.
Further, step S3 is performed 3-6 times.
Further, the preset mass ratio is 1-2: 5-10.
Further, the preset rotating speed is 300rpm-500 rpm; the first preset time is 30min-60 min.
Further, step S2 includes:
s21: closing the micro-jet homogenizer and opening the high-pressure homogenizer;
s22: adding the nano particle slurry into a high-pressure homogenizer through a feed inlet;
s23: adjusting the rotation speed of the high-pressure homogenizer to 400-500 rpm, and preheating the high-pressure homogenizer at the rotation speed;
s24: setting the working pressure of the high-pressure homogenizer to be 1500bar-1800 bar;
s25: the nano particle slurry flows into a working valve gap of the high-pressure homogenizer from the feeding hole to be extruded, and the extrusion pressure between the working valve gaps is adjusted to keep the same as the working pressure of the high-pressure homogenizer;
s26: and after the working time of the high-pressure homogenizer reaches the second preset time, collecting the nano particle slurry flowing out of the discharge hole of the high-pressure homogenizer, and closing the high-pressure homogenizer.
Further, the second preset time is 30-60 min.
Further, step S3 includes:
s31: opening a switch of the micro-jet homogenizer, and adjusting the working pressure of the micro-jet homogenizer to be 1500bar-1800 bar;
s32: adding the nano particle slurry obtained by shearing in the step S2 into a homogenizing cavity of a micro-jet homogenizer through a feed inlet;
s33: and (3) carrying out secondary shearing on the nanoparticle slurry in a homogenizing cavity of the micro-jet homogenizer, leading out the obtained stably dispersed nanoparticle aqueous dispersion liquid after the working time of the micro-jet homogenizer reaches a third preset time, and closing the micro-jet homogenizer.
Further, the third preset time is 30-60 min.
Further, the homogenizing chamber of the micro-jet homogenizer is made of artificial diamond.
The invention aims to provide a method for preparing nano particle slurry, which comprises the steps of mixing raw material nano particles and water according to a preset mass ratio, and then mechanically stirring at a preset rotating speed within a first preset time to obtain nano particle slurry; adding the nano particle slurry into a high-pressure homogenizer for shearing so as to reduce the particle size of the nano particles in the nano particle slurry; and finally, adding the sheared nanoparticle slurry into a micro-jet homogenizer for secondary shearing to obtain a nanoparticle aqueous dispersion, wherein the particle size of the nanoparticles in the nanoparticle aqueous dispersion is 50-300 nm. The nano particle aqueous dispersion is prepared by shearing with a high-pressure homogenizer and secondary shearing with a micro-jet homogenizer, and the size of nano particles can be controlled by adjusting the pressure and the processing time of the shearing with the high-pressure homogenizer and the micro-jet homogenizer in the preparation process, so that the prepared nano particle aqueous dispersion has good stability and can be stably placed for one month or more.
(III) advantageous effects
The technical scheme of the invention has the following beneficial technical effects: the adopted method is simple, does not need to use an organic solvent and a stabilizer, and does not have the problems of environmental pollution and subsequent waste liquid treatment; the nanoparticle dispersion liquid is prepared through pretreatment of a high-pressure homogenizer and secondary treatment of a micro-jet homogenizer, the size of the nanoparticles can be controlled by adjusting the pressure of equipment and the treatment time in the preparation process, the prepared dispersion liquid is good in stability and can be stably placed for one month or more, water is used as a dispersing agent, the application range is wider, a simple and efficient method is provided for preparation of the nanoparticle stable dispersion liquid, and the method is easy to popularize in a large range.
The method is simple, does not need to use organic solvent and stabilizer, and does not have the problems of environmental pollution and subsequent waste liquid treatment.
The dispersion medium is water, the water is a common dispersion medium in production, and particularly the nano-particle oil displacement agent in petroleum tertiary recovery generally adopts the water as the dispersion medium.
Drawings
FIG. 1 is a flow chart of a method of preparation provided by the present invention;
FIG. 2 is a flow chart of step S2 of the preparation method provided by the present invention;
fig. 3 is a flowchart of step S3 of the preparation method provided by the present invention.
Reference numerals:
the method comprises the following steps: s1; s2; s3; s21; s22; s23; s24; s25; s26; s31; s32; and S32.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
The present invention will be described in detail below with reference to the accompanying drawings and examples.
FIG. 1 is a flow chart of a preparation method provided by the present invention.
In one embodiment, the present invention provides a method for preparing an aqueous dispersion of nanoparticles, comprising the steps of:
s1: mixing raw material nanoparticles and water according to a preset mass ratio, and mechanically stirring at a preset rotating speed for a first preset time to obtain nanoparticle slurry;
s2: adding the nano particle slurry into a high-pressure homogenizer for shearing so as to reduce the particle size of the nano particles in the nano particle slurry;
s3: and adding the sheared nanoparticle slurry into a micro-jet homogenizer for secondary shearing to obtain a nanoparticle aqueous dispersion, wherein the particle size of the nanoparticles in the nanoparticle aqueous dispersion is 50-300 nm.
Specifically, in step S1, the raw material nanoparticles and water are mixed according to a preset mass ratio of 1-2: 5-10. Preferably, the preset mass ratio is 2:8, the mud flow property of the mass ratio is good, an instrument cannot be blocked, and the treatment effect is better compared with that of high-concentration nano particles.
Optionally, the raw material nanoparticles include graphene, graphene oxide, modified graphene, nanocellulose, nano titanium dioxide, and the like. The nanometer material has low viscosity, and can prevent the blockage of instruments and other problems.
In one embodiment, the preset rotation speed is 300rpm to 500rpm, and the raw material nanoparticles can be fully contacted with water by stirring at the preset rotation speed; preferably, the preset rotation speed is 400 rpm.
The first preset time is 30min-60min, and the raw material nano particles can be fully wetted by water by stirring within the preset time range; preferably, the first preset time is 60 min.
Fig. 2 is a flowchart of step S2 of the preparation method provided by the present invention.
In one embodiment, step S2 includes:
s21: and (4) closing the micro-jet homogenizer and opening the high-pressure homogenizer.
S22: and adding the nano particle slurry into a high-pressure homogenizer through a feed inlet.
S23: the rotating speed of the high-pressure homogenizer is adjusted to be 400rpm-500rpm, so that the high-pressure homogenizer is preheated at the rotating speed.
S24: the working pressure of the high-pressure homogenizer is set to be 1500bar-1800 bar.
S25: and (3) allowing the nano particle slurry to flow into a working valve gap of the high-pressure homogenizer from the feeding hole for extrusion, and adjusting the extrusion pressure between the working valve gaps to keep the same as the working pressure of the high-pressure homogenizer.
S26: and after the working time of the high-pressure homogenizer reaches the second preset time, collecting the nano particle slurry flowing out of the discharge hole of the high-pressure homogenizer, and closing the high-pressure homogenizer.
Specifically, in step S21, the high-pressure homogenizer and the micro-jet homogenizer are integrated machines, and can be controlled by different switches to operate respectively. The high-pressure homogenizer and the microjet homogenizer share the same feed inlet, and when the high-pressure homogenizer is used for shearing, a valve between the feed inlet and the microjet homogenizer needs to be closed at first, so that the nano particle slurry is prevented from entering the microjet homogenizer.
In step S23, the rotor speed of the high-pressure homogenizer needs to be adjusted to 400rpm-500rpm, the rotation speed is adjusted to make the reciprocating pump of the high-pressure homogenizer work in advance, and the rotation speed range can play a role of preheating the machine; preferably, the rotor speed of the high-pressure homogenizer is adjusted to 450 rpm.
In step S24, the pressure of the high-pressure homogenizer needs to be set in advance before shearing the nanoparticle slurry. In the embodiment, the working pressure of the high-pressure homogenizer is adjusted to be 1500-1800 bar by a manual booster valve of the high-pressure homogenizer; the pressure range can reduce the particle size of the nano particles in a shorter time range; preferably, the working pressure is 1700 bar.
In step S25, the nanoparticle slurry flows into the work valve gap of the high-pressure homogenizer through the feed port, and is extruded in the work valve gap. The extrusion pressure of the working valve gap can be changed due to the mutual extrusion of the particles, and at the moment, the extrusion pressure of the nano particles between the working valve gap is kept consistent with the previously set working pressure of the high-pressure homogenizer through manual adjustment, so that the particle size of the nano particles can be uniformly reduced.
When the nano particle slurry passes through the gap of the working valve, the nano particle slurry is subjected to very low pressure, the pressure is generally 1bar, so that the nano particle slurry subjected to instantaneous pressure loss can generate a void effect, and the nano particle slurry is ejected at a very high speed, so that a strong impact force is generated. The nano particle slurry can generate a certain shearing force among the nano particles in the high-speed spraying process, and the shearing force can reduce the particle size of the nano particles and uniformly disperse the nano particles in water.
In one embodiment, the second predetermined time is 30min-60 min.
Specifically, the high-pressure homogenization time is 30min-60min, and the time can realize the primary shearing process of the nanoparticles; preferably, the second preset time is 30 min.
In step S26, the sheared nanoparticle slurry flows out of the discharge port of the high-pressure homogenizer, the sheared nanoparticle slurry is collected together, the high-pressure homogenizer needs to be washed by deionized water, the switch of the high-pressure homogenizer is closed until the outlet of the high-pressure homogenizer is clean and free of impurities, and the rotation speed of the rotor of the high-pressure homogenizer is adjusted to 0.
In one embodiment, step S2 is performed 3-6 times.
Specifically, the particle size of the nanoparticles can be controlled by adjusting the pressure and shearing time of the high-pressure homogenizer, while also being related to the number of treatments. The more times the nanoparticle slurry is processed in the high-pressure homogenizer, the smaller the particle size of the nanoparticles after shearing, the less times the nanoparticle slurry is processed in the high-pressure homogenizer, and the larger the particle size of the nanoparticles after shearing. In this embodiment, the number of times the nanoparticle slurry is treated in the high-pressure homogenizer is preferably 3 to 6 times.
Fig. 3 is a flowchart of step S3 of the preparation method provided by the present invention.
In one embodiment, step S3 includes:
s31: and opening a switch of the micro-jet homogenizer, and adjusting the working pressure of the micro-jet homogenizer to be 1500bar-1800 bar.
S32: and (4) adding the nanoparticle slurry obtained by shearing in the step S2 into a homogenizing cavity of the microfluid homogenizer through a feed inlet.
S33: and (3) carrying out secondary shearing on the nanoparticle slurry in a homogenizing cavity of the micro-jet homogenizer, leading out the obtained stably dispersed nanoparticle aqueous dispersion liquid after the working time of the micro-jet homogenizer reaches a third preset time, and closing the micro-jet homogenizer.
Specifically, in step S32, the switch of the micro-fluidic homogenizer is turned on, and the operating pressure of the micro-fluidic homogenizer is adjusted to 1500bar-1800bar by the pressure adjusting knob of the micro-fluidic homogenizer. Under the pressure range, the particle size of the nano particles can be reduced in a shorter time range; preferably, the operating pressure of the microfluidizer is 1700 bar.
In step S31, the valve between the inlet and the high-pressure homogenizer is closed, and the nanoparticle slurry collected in step S26 is added into the homogenizing chamber of the microfluidizer through the inlet.
In step S33, the microfluidizer mainly comprises a homogenizing chamber and a pressurizing mechanism, a "Z" channel is arranged inside the homogenizing chamber, and under the action of the pressurizing mechanism, the nanoparticle slurry under high pressure rapidly passes through the homogenizing chamber, and is jetted in the opposite direction, and is collided at high speed. The nano particle slurry is subjected to the actions of shearing force, high-frequency oscillation, cavity effect and impact effect in the process, so that secondary shearing and crushing of the nano particle slurry are realized.
And collecting a product flowing out of a discharge hole of the micro-jet homogenizer to obtain the stably dispersed nano particle aqueous dispersion, wherein the size of nano particles in the nano particle aqueous dispersion is 50-300nm, and the nano particle aqueous dispersion can be stably placed for more than one month without agglomeration and sedimentation.
In one embodiment, the third predetermined time is 30min-60 min.
Specifically, the microjet homogenization time is 30min-60min, and the time range can realize effective reduction of the particle size of the nanoparticles; preferably, the third predetermined time is 60 min.
In one embodiment, step S3 is performed 3-6 times.
In particular, the nanoparticle size can be controlled by adjusting the pressure and shear time of the microfluidizer, while also being related to the number of treatments. The more times the nanoparticle slurry is processed in the microfluidizer, the smaller the particle size of the sheared nanoparticles, the less times the nanoparticle slurry is processed in the microfluidizer, and the larger the particle size of the sheared nanoparticles. In this embodiment, the number of times the nanoparticle slurry is treated in the microfluidizer is preferably 3 to 6 times.
In one embodiment, the homogenizing chamber of the microfluidizer is made of synthetic diamond.
Specifically, the diamond material is harder, and can avoid the conditions of equipment cracking, chipping and the like during particle collision so as to avoid polluting products. Meanwhile, the artificial diamond has lower cost and is more economical than natural diamond.
The first embodiment is as follows:
step 1: mixing the graphene nanoparticles with water according to a mass ratio of 1: 5; and mechanically stirring the mixed graphene nano particles and water to prepare graphene nano particle slurry, wherein the stirring speed is 400 revolutions per minute, and the stirring time is 60 min.
Step 2: shearing the graphene nanoparticle slurry: firstly, closing a switch of the micro-jet homogenizer, and then opening a switch of the high-pressure homogenizer; adding into a feed inlet; regulating the rotating speed of a rotor of the high-pressure homogenizer to 450 revolutions per minute; adjusting the working pressure of the high-pressure homogenizer to 1500 bar; the high pressure homogenization time is 30 min.
And step 3: repeat step 23 times.
And 4, step 4: and (3) collecting the graphene nano particle slurry pretreated in the step (3), washing the high-pressure homogenizer by using deionized water, closing a switch of the high-pressure homogenizer until the discharged liquid from the discharge hole is clean and has no impurities, and adjusting the rotating speed of the rotor to 0.
And 5: carrying out secondary shearing on the graphene nano particle slurry: opening a switch of the micro-jet homogenizer; adding the graphene nano particle slurry collected in the step 4 into a feed inlet; adjusting the working pressure of the micro-jet homogenizer to 1600 bar; the microfluid homogenization time is 60 min.
Step 6: repeat step 5 3 times.
And 7: and (4) collecting the product treated in the step (6), namely obtaining the graphene nanoparticle aqueous dispersion liquid which is stably dispersed, measuring the particle size range of the nanoparticles to be 120-280nm by using a laser particle sizer, and stably placing for one month without precipitation.
Example two:
step 1: mixing the graphene nanoparticles with water according to a mass ratio of 1: 5; and mechanically stirring the mixed graphene nano particles and water to prepare graphene nano particle slurry, wherein the stirring speed is 400 revolutions per minute, and the stirring time is 60 min.
Step 2: shearing the graphene nanoparticle slurry: firstly, closing a switch of the micro-jet homogenizer, and then opening a switch of the high-pressure homogenizer; adding into a feed inlet; regulating the rotating speed of a rotor of the high-pressure homogenizer to 450 revolutions per minute; adjusting the working pressure of the high-pressure homogenizer to 1500 bar; the high pressure homogenization time is 30 min.
And step 3: repeat step 24 times.
And 4, step 4: collecting the graphene nano particle slurry pretreated in the step 3 together; washing the high-pressure homogenizer by deionized water, and turning off the switch of the high-pressure homogenizer until the liquid discharged from the discharge hole is clean and has no impurities, so as to adjust the rotating speed of the rotor to 0.
And 5: carrying out secondary shearing on the graphene nano particle slurry: opening a switch of the micro-jet homogenizer; adding the graphene nano particle slurry collected in the step 4 into a feed inlet; adjusting the working pressure of the micro-jet homogenizer to 1600 bar; the microfluid homogenization time is 60 min.
Step 6: repeat step 5 4 times.
And 7: and (4) collecting the product treated in the step (6), namely obtaining the stably dispersed graphene nanoparticle aqueous dispersion, measuring the particle size range of the nanoparticles by using a laser particle sizer to be 80-200nm, and stably storing for one week without precipitation.
Example three:
step 1: mixing the graphene nanoparticles with water according to a mass ratio of 1: 5; and mechanically stirring the mixed graphene nano particles and water to prepare graphene nano particle slurry, wherein the stirring speed is 400 revolutions per minute, and the stirring time is 60 min.
Step 2: shearing the graphene nanoparticle slurry: firstly, closing a switch of the micro-jet homogenizer, and then opening a switch of the high-pressure homogenizer; adding into a feed inlet; regulating the rotating speed of a rotor of the high-pressure homogenizer to 450 revolutions per minute; adjusting the working pressure of the high-pressure homogenizer to 1500 bar; the high pressure homogenization time is 30 min.
And step 3: repeat step 26 times.
And 4, step 4: collecting the graphene nano particle slurry pretreated in the step 3 together; washing the high-pressure homogenizer by deionized water, and turning off the switch of the high-pressure homogenizer until the liquid discharged from the discharge hole is clean and has no impurities, so as to adjust the rotating speed of the rotor to 0.
And 5: carrying out secondary shearing on the graphene nano particle slurry: opening a switch of the micro-jet homogenizer; adding the graphene nano particle slurry collected in the step 4 into a feed inlet; the working pressure of the micro-jet homogenizer is adjusted to 1600bar by an adjusting knob; the microfluid homogenization time is 60 min.
Step 6: repeat step 5 6 times.
And 7: and (4) collecting the product treated in the step (6), namely obtaining the graphene nanoparticle aqueous dispersion liquid which is stably dispersed, measuring the particle size range of the nanoparticles to be 50-160nm by using a laser particle sizer, and stably storing for one week without precipitation.
Example four:
step 1: mixing the graphene nanoparticles with water, wherein the mass ratio of the graphene nanoparticles to the water is 2: 8; and mechanically stirring the mixed graphene nano particles and water to prepare graphene nano particle slurry, wherein the stirring speed is 400 revolutions per minute, and the stirring time is 60 min.
Step 2: shearing the graphene nanoparticle slurry: firstly, closing a switch of the micro-jet homogenizer, and then opening a switch of the high-pressure homogenizer; adding into a feed inlet; regulating the rotating speed of a rotor of the high-pressure homogenizer to 450 revolutions per minute; adjusting the working pressure of the high-pressure homogenizer to 1600 bar; the high pressure homogenization time is 30 min.
And step 3: repeat step 24 times.
And 4, step 4: collecting the graphene nano particle slurry pretreated in the step 3 together; washing the high-pressure homogenizer by deionized water, and turning off the switch of the high-pressure homogenizer until the liquid discharged from the discharge hole is clean and has no impurities, so as to adjust the rotating speed of the rotor to 0.
And 5: carrying out secondary shearing on the graphene nano particle slurry: opening a switch of the micro-jet homogenizer; adding the graphene nano particle slurry collected in the step 4 into a feed inlet; the working pressure of the microjet homogenizer is regulated to 1700bar by the regulating knob; the microfluidization homogenization time was 30 min.
Step 6: repeat step 5 6 times.
And 7: and (4) collecting the product treated in the step (6), namely obtaining the stably dispersed graphene nanoparticle aqueous dispersion, measuring the particle size range of the nanoparticles by using a laser particle sizer to be 80-270nm, and stably storing for one week without precipitation.
Example five:
step 1: mixing the graphene nanoparticles with water, wherein the mass ratio of the graphene nanoparticles to the water is 2: 8; and mechanically stirring the mixed graphene nano particles and water to prepare graphene nano particle slurry, wherein the stirring speed is 400 revolutions per minute, and the stirring time is 60 min.
Step 2: shearing the graphene nanoparticle slurry: firstly, closing a switch of the micro-jet homogenizer, and then opening a switch of the high-pressure homogenizer; adding into a feed inlet; regulating the rotating speed of a rotor of the high-pressure homogenizer to 450 revolutions per minute; adjusting the working pressure of the high-pressure homogenizer to 1600 bar; the high pressure homogenization time is 60 min.
And step 3: repeat step 24 times.
And 4, step 4: collecting the graphene nano particle slurry pretreated in the step 3 together; washing the high-pressure homogenizer by deionized water, and turning off the switch of the high-pressure homogenizer until the liquid discharged from the discharge hole is clean and has no impurities, so as to adjust the rotating speed of the rotor to 0.
And 5: carrying out secondary shearing on the graphene nano particle slurry: opening a switch of the micro-jet homogenizer; adding the graphene nano particle slurry collected in the step 4 into a feed inlet; the working pressure of the microjet homogenizer is regulated to 1700bar by the regulating knob; the microfluid homogenization time is 60 min.
Step 6: repeat step 5 6 times.
And 7: and (3) collecting the product treated in the step (6), namely obtaining the graphene nanoparticle aqueous dispersion with stable dispersion, wherein the particle size range of the nanoparticles measured by a laser particle sizer is as follows: 50-140nm, stable storage for one week without precipitation.
The invention aims to protect a preparation method of a nanoparticle aqueous dispersion, which comprises the following steps: mixing raw material nanoparticles and water according to a preset mass ratio, and mechanically stirring at a preset rotating speed for a first preset time to obtain nanoparticle slurry; adding the nano particle slurry into a high-pressure homogenizer for shearing so as to reduce the particle size of the nano particles in the nano particle slurry; and finally, adding the sheared nanoparticle slurry into a micro-jet homogenizer for secondary shearing to obtain a nanoparticle aqueous dispersion, wherein the particle size of the nanoparticles in the nanoparticle aqueous dispersion is 50-300 nm. The nano particle aqueous dispersion is prepared by shearing with a high-pressure homogenizer and secondary shearing with a micro-jet homogenizer, and the size of nano particles can be controlled by adjusting the pressure and the processing time of the shearing with the high-pressure homogenizer and the micro-jet homogenizer in the preparation process, so that the prepared nano particle aqueous dispersion has good stability and can be stably placed for one month or more. The method is simple, does not need to use organic solvent and stabilizer, does not have the problems of environmental pollution and subsequent waste liquid treatment, provides a simple and efficient method for preparing the stable dispersion liquid of the nanoparticles, and is easy to popularize in a large range.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (9)
1. A method for preparing an aqueous dispersion of nanoparticles, comprising:
s1: mixing raw material nanoparticles and water according to a preset mass ratio, and mechanically stirring at a preset rotating speed for a first preset time to obtain nanoparticle slurry;
s2: adding the nanoparticle slurry into a high-pressure homogenizer for shearing to reduce the particle size of the nanoparticles in the nanoparticle slurry, wherein the shearing comprises the following steps:
the nano particle slurry flows into a working valve gap of the high-pressure homogenizer from a feed inlet to be extruded, and the extrusion pressure between the working valve gaps is adjusted to keep the same as the working pressure of the high-pressure homogenizer;
after the working time of the high-pressure homogenizer reaches a second preset time, nano particle slurry subjected to primary shearing is obtained;
s3: adding the sheared nano particle slurry into a micro-jet homogenizer for secondary shearing to obtain a nano particle aqueous dispersion, wherein the particle size of nano particles in the nano particle aqueous dispersion is 50-300 nm;
wherein the preset mass ratio is 1-2: 5-10.
2. The production method according to claim 1,
step S2 is performed 3-6 times.
3. The production method according to claim 1 or 2,
step S3 is performed 3-6 times.
4. The production method according to claim 1,
the preset rotating speed is 300-500 rpm;
the first preset time is 30-60 min.
5. The method as claimed in claim 1 or 2, wherein the step S2 is further performed before the step S2 of flowing the nanoparticle slurry from the inlet into a working valve gap of the high-pressure homogenizer for extrusion, and adjusting the extrusion pressure between the working valve gap to be consistent with the working pressure of the high-pressure homogenizer:
s21: closing the micro-jet homogenizer and opening the high-pressure homogenizer;
s22: adding the nanoparticle slurry into the high-pressure homogenizer through a feed inlet;
s23: adjusting the rotation speed of the high-pressure homogenizer to be 400-500 rpm, and preheating the high-pressure homogenizer at the rotation speed;
s24: the working pressure of the high-pressure homogenizer is set to be 1500bar-1800 bar.
6. The production method according to claim 1,
the second preset time is 30-60 min.
7. The method for preparing a composite material according to claim 1, wherein the step S3 includes:
s31: opening a switch of the micro-jet homogenizer, and adjusting the working pressure of the micro-jet homogenizer to be 1500bar-1800 bar;
s32: adding the nanoparticle slurry obtained by shearing in the step S2 into a homogenizing cavity of the micro-jet homogenizer through a feed inlet;
s33: and carrying out secondary shearing on the nanoparticle slurry in a homogenizing cavity of the micro-jet homogenizer, leading out the obtained stably dispersed nanoparticle aqueous dispersion after the working time of the micro-jet homogenizer reaches a third preset time, and closing the micro-jet homogenizer.
8. The production method according to claim 7,
the third preset time is 30-60 min.
9. The production method according to claim 1 or 7,
the homogenizing cavity of the micro-jet homogenizer is made of artificial diamond.
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