CN110124548A - A kind of preparation method of nanoparticle aqueous dispersions - Google Patents
A kind of preparation method of nanoparticle aqueous dispersions Download PDFInfo
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- CN110124548A CN110124548A CN201910320223.9A CN201910320223A CN110124548A CN 110124548 A CN110124548 A CN 110124548A CN 201910320223 A CN201910320223 A CN 201910320223A CN 110124548 A CN110124548 A CN 110124548A
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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
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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
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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 kind of preparation method of nanoparticle aqueous dispersions, comprising: after mixing raw material nano particle by preset quality proportion with water, carry out mechanical stirring in preset rotation speed and the first preset time, obtain nanoparticle slurry；Nanoparticle slurry addition high pressure homogenizer is sheared again, to reduce nano particle diameter in nanoparticle slurry；Microfluidizer finally is added in the nanoparticle slurry after shearing and carries out secondary shearing, obtains nanoparticle aqueous dispersions, wherein the partial size of nanoparticle is 50-300nm in nanoparticle aqueous dispersions.It carries out preparing nanoparticle aqueous dispersions by high pressure homogenizer shearing and Microfluidizer secondary shearing, preparation process is by adjusting the pressure of high pressure homogenizer shearing and Microfluidizer and handling the time, it can control nano-particles size, so that the nanoparticle aqueous dispersions stability of preparation is preferable.This method is simple, does not need that environmental pollution and subsequent liquid waste processing problem is not present using organic solvent and stabilizer.
Description
Technical field
The present invention relates to nanoparticle technical field, in particular to a kind of preparation method of nanoparticle aqueous dispersions.
Background technique
The size of nanoparticle has a major impact its physical attribute and chemical characteristic, and nanoparticle is imitated due to its small size
It answers, skin effect and quantum size effect etc. have physical properties and the chemical properties such as many excellent electricity, light, magnetic, power, heat.
In many production technologies, it is desirable that nanoparticle is uniformly and stably dispersed in liquid phase medium, such as: paint, medicine, dyestuff
With cosmetics preparation etc.；In recent years, whether nanoparticle oil displacement agent used in adopting in petroleum three can uniformly divide in an aqueous medium
It dissipates and nano-particles size will directly affect the effect of its application at the scene.
However, nanoparticle due to specific surface area greatly, surface can be higher, the nanoparticle to float on a liquid has mutual
Mutually reunite to reduce the trend of its surface energy, can do random Brownian movement between the nanoparticle furthermore to suspend and mutually touch
It hits to form aggregate, leads to the reduction of nanoparticle dispersion degree, while aggregate settles under the effect of gravity, nano suspending liquid is stablized
Property therefore decline.Therefore, reduce the collision frequency and agglomeration tendency in nano suspending liquid between nanoparticle, keep nanoparticle uniform
Disperse and stable suspersion in base fluid, is ultimately forming evenly dispersed, suspending stabilized nano suspending liquid as research hotspot.
According to the difference of dispersing method, the method for improving nano suspending liquid stability can be divided into physical dispersion method and chemistry
Dispersion method, physical dispersion method mainly include ultrasonic disperse and mechanical dispersion, and chemical dispersion method mainly includes addition dispersing agent, adjusts
PH of suspension, nano particle surface modifying etc..
Ultrasonic dispersion is so that liquid is generated cavitation using the dispersion effect of ultrasonic wave in a liquid and make in physical method
With, to make in liquid solid particle broken, increase the method for dispersion stable, in ultrasonication, often with compared with
Big noise, product cut size is uneven after processing；Mechanical dispersion is that the impact force generated by mechanical equipment or shearing force etc. make
A kind of method of nanoparticle dispersion, wherein commonly Ball Milling and mechanical stirring dispersion method, Ball Milling can be with
Keep nanoparticle broken, partial size is made to become smaller, increases dispersion stability.But in ball milling dispersion process, sphere and mill tube are easy to produce
Raw abrasion substance, influences nano material purity；Mechanical stirring carries out nanoparticle suspension generally by magnetic agitation etc.
Lasting stirring, makes nanoparticle float on a liquid, achievees the effect that dispersion, once stopping stirring, nanoparticle has to be gathered again
Collection, causes nanoparticle dispersion system to cannot keep stable dispersion state.
A kind of preparation method of the rutile type nano titanic oxide particle of size tunable, including with perchloric acid and isopropanol
Titanium prepares titanium dioxide crystal seed, rear to prepare rutile nanoparticles, the nanoparticle seed prepared in the present invention by hydro-thermal reaction
Diameter is controllable, uniformity and good dispersion, belongs to nano particle surface modifying in chemical dispersion method, and preparation process will use a variety ofization
Reagent is learned, reaction process temperature is relatively high, and the time is long, has certain risk, is not suitable for large-scale production preparation.
A method of graphene being prepared, this method prepares feedstock solution by making expanded graphite high speed homogenisation, so
After make the feedstock solution high pressure homogenizing, to improve high pressure by improving expanded graphite dispersibility in the feed solution
Homogenize efficiency.The graphene method prepared in the present invention is simple, of uniform size, and method used in the present invention belongs to physics point
Mechanical dispersion in arching pushing, process is fairly simple, but in invention in order to improve expanded graphite and graphene dispersion degree used it is a variety of
Dispersing agent maintains its dispersity, affects the purity of product itself.
Although disclosing the method for much preparing nanoparticle dispersion liquid at present, size controlling is can be achieved in part, wherein changing
Method is related to the use of many organic solvents and chemical reagent, and there are environmental pollution and some potential safety problems, part chemistry changes
Property just for specific nanoparticle and functional group, there is significant limitation；In comparison, physical method is more environmentally friendly, safety,
But the problems such as that there are dispersion efficiencies is low for physical method, and the processing time is long, and equipment energy consumption is high, therefore on the basis of existing, find one kind
Efficiently, environmentally friendly, dispersing method applied widely is of great significance to the application of nanoparticle dispersion liquid.
Summary of the invention
(1) goal of the invention
The object of the present invention is to provide a kind of preparation method of nanoparticle aqueous dispersions, by high pressure homogenizer shearing and
Microfluidizer secondary shearing prepare nanoparticle aqueous dispersions, preparation process by adjust high pressure homogenizer shearing and
The pressure of Microfluidizer and processing time, it can control the size of nanoparticle, so that the nanoparticle aqueous dispersions of preparation
Stability is good, can stablize placement one month or more.
(2) technical solution
To solve the above problems, according to an aspect of the present invention, the present invention provides a kind of nanoparticle aqueous dispersions
Preparation method, comprising:
S1: after raw material nano particle is mixed with water by preset quality proportion, in preset rotation speed and the first preset time
Mechanical stirring is carried out, nanoparticle slurry is obtained；
S2: nanoparticle slurry addition high pressure homogenizer is sheared, to reduce nanoparticle in nanoparticle slurry
Partial size；
S3: Microfluidizer is added in the nanoparticle slurry after shearing and carries out secondary shearing, obtains nanoparticle water
Dispersion liquid, wherein the partial size of nanoparticle is 50-300nm in nanoparticle aqueous dispersions.
Further, step S2 is executed 3-6 times.
Further, step S3 is executed 3-6 times.
Further, preset quality proportion is 1-2:5-10.
Further, preset rotation speed 300rpm-500rpm；First preset time is 30min-60min.
Further, step S2 includes:
S21: closing Microfluidizer, opens high pressure homogenizer；
S22: nanoparticle slurry is added in high pressure homogenizer by feed inlet；
S23: the revolving speed for adjusting high pressure homogenizer is 400rpm-500rpm, carries out high pressure homogenizer under the revolving speed in advance
Heat；
S24: the operating pressure of high pressure homogenizer is set as 1500bar-1800bar；
S25: nanoparticle slurry is squeezed from the operating valve gap that feed inlet flows into high pressure homogenizer, adjusts work
Squeeze pressure between valve gap is consistent the operating pressure of itself and high pressure homogenizer；
S26: after the working time of high pressure homogenizer reached for the second predetermined time, the discharge port stream of high pressure homogenizer is collected
Nanoparticle slurry out closes high pressure homogenizer.
Further, the second preset time is 30min-60min.
Further, step S3 includes:
S31: opening Microfluidizer switch, and the operating pressure for adjusting Microfluidizer is 1500bar-1800bar；
S32: the homogeneous chamber of Microfluidizer is added by feed inlet for the nanoparticle slurry that step S2 is sheared
In；
S33: nanoparticle slurry carries out secondary shearing in the homogeneous chamber of Microfluidizer, in Microfluidizer work
After reaching the third predetermined time as the time, the nanoparticle aqueous dispersions of obtained stable dispersion are exported, and close microjet
Homogenizer.
Further, the third predetermined time is 30min-60min.
Further, the homogeneous chamber of Microfluidizer is made of diamond.
The object of the present invention is to provide it is a kind of raw material nano particle and water mixs by preset quality proportion after, at default turn
Mechanical stirring is carried out in speed and the first preset time, obtains nanoparticle slurry；Nanoparticle slurry is added again high-pressure homogeneous
Machine is sheared, to reduce nano particle diameter in nanoparticle slurry；Finally the nanoparticle slurry after shearing is added micro-
Jet homogenizer carries out secondary shearing, obtains nanoparticle aqueous dispersions, wherein nanoparticle in nanoparticle aqueous dispersions
Partial size is 50-300nm.It carries out preparing nanoparticle water dispersion by high pressure homogenizer shearing and Microfluidizer secondary shearing
Liquid, preparation process can control nanoparticle by adjusting the pressure of high pressure homogenizer shearing and Microfluidizer and handling the time
The size of son can be stablized placement one month or more so that the nanoparticle aqueous dispersions stability of preparation is good.
(3) beneficial effect
Above-mentioned technical proposal of the invention has following beneficial technical effect: the method for use is simple, do not need using
Environmental pollution and subsequent liquid waste processing problem is not present in organic solvent and stabilizer；It is penetrated by high pressure homogenizer pretreatment with micro-
Stream homogenizer secondary treatment prepares nanoparticle dispersion liquid, and preparation process is received by the way that adjustment equipment pressure and processing time are controllable
The dispersion stability of rice corpuscles size, preparation is good, can stablize placement one month or more, using water as dispersing agent, using model
It encloses more extensively, provides one simply for the preparation of nanoparticle stable dispersions, efficient method is easy to promote on a large scale.
The method of use is simple, does not need using organic solvent and stabilizer, there is no at environmental pollution and subsequent waste liquid
Reason problem.
Decentralized medium is water, and water is to commonly use decentralized medium, especially petroleum three in production to adopt middle nanoparticle oil displacement agent general
All over use water as decentralized medium.
Detailed description of the invention
Fig. 1 is the flow chart of preparation method provided by the invention；
Fig. 2 is the flow chart of the step S2 of preparation method provided by the invention；
Fig. 3 is the flow chart of the step S3 of preparation method provided by the invention.
Appended drawing reference:
Step: S1；S2；S3；S21；S22；S23；S24；S25；S26；S31；S32；S32.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment and join
According to attached drawing, the present invention is described in more detail.It should be understood that these descriptions are merely illustrative, and it is not intended to limit this hair
Bright range.In addition, in the following description, descriptions of well-known structures and technologies are omitted, to avoid this is unnecessarily obscured
The concept of invention.
The present invention is described in detail with reference to the accompanying drawings and examples.
Fig. 1 is the flow chart of preparation method provided by the invention.
In one embodiment, the present invention provides a kind of preparation methods of nanoparticle aqueous dispersions, comprising the following steps:
S1: after raw material nano particle is mixed with water by preset quality proportion, in preset rotation speed and the first preset time
Mechanical stirring is carried out, nanoparticle slurry is obtained；
S2: nanoparticle slurry addition high pressure homogenizer is sheared, to reduce nanoparticle in nanoparticle slurry
Partial size；
S3: Microfluidizer is added in the nanoparticle slurry after shearing and carries out secondary shearing, obtains nanoparticle water
Dispersion liquid, wherein the partial size of nanoparticle is 50-300nm in nanoparticle aqueous dispersions.
Specifically, in step S1, by raw material nano particle and water by preset quality proportion mixing, preset quality proportion is 1-
2:5-10.Preferably, preset quality proportion is 2:8, and the quality proportioning slip fluidity is good, will not block instrument, compared to highly concentrated
Nanoparticle is spent, treatment effect is more preferable.
Optionally, raw material nano particle includes graphene, graphene oxide, modified graphene, nano-cellulose, nanometer two
Titanium oxide etc..Above-mentioned nano material viscosity is lower, can prevent the problems such as causing instrument to block.
In one embodiment, preset rotation speed 300rpm-500rpm is stirred under the preset rotation speed, can make original
Material nanoparticle comes into full contact with water；Preferably, preset rotation speed 400rpm.
First preset time is 30min-60min, is stirred in the preset time range, can make raw material nano particle
Sufficiently it is spontaneously wet out by water；Preferably, the first preset time is 60min.
Fig. 2 is the flow chart of the step S2 of preparation method provided by the invention.
In one embodiment, step S2 includes:
S21: closing Microfluidizer, opens high pressure homogenizer.
S22: nanoparticle slurry is added in high pressure homogenizer by feed inlet.
S23: the revolving speed for adjusting high pressure homogenizer is 400rpm-500rpm, carries out high pressure homogenizer under the revolving speed in advance
Heat.
S24: the operating pressure of high pressure homogenizer is set as 1500bar-1800bar.
S25: nanoparticle slurry is squeezed from the operating valve gap that feed inlet flows into high pressure homogenizer, adjusts work
Squeeze pressure between valve gap is consistent the operating pressure of itself and high pressure homogenizer.
S26: after the working time of high pressure homogenizer reached for the second predetermined time, the discharge port stream of high pressure homogenizer is collected
Nanoparticle slurry out closes high pressure homogenizer.
Specifically, in step S21, high pressure homogenizer and Microfluidizer are integrated machine, can pass through different switches
Control makes it work respectively, and in an embodiment of the present invention, high pressure homogenizer and Microfluidizer work independently, can not
It works at the same time.High pressure homogenizer and Microfluidizer are used in conjunction with the same feed inlet, are cut using high pressure homogenizer
When cutting, it is necessary first to close the valve between feed inlet and Microfluidizer, prevent nanoparticle slurry from entering microjet equal
In matter machine.
In step S23, the rotor speed for needing first to adjust high pressure homogenizer is 400rpm-500rpm, and first adjusting revolving speed is
In order to make the reciprocating pump of high pressure homogenizer work together in advance, the above-mentioned range of speeds can play the role of warming up machinery；It is preferred that
, the rotor speed for adjusting high pressure homogenizer is 450rpm.
In step S24, before carrying out shearing nanoparticle slurry, need to preset the pressure of high pressure homogenizer.This
In embodiment, the operating pressure by the hand supercharging valve regulation high pressure homogenizer of high pressure homogenizer is 1500bar-1800bar；
The pressure limit can make nano particle diameter reduce within the short period；Preferably, operating pressure 1700bar.
In step S25, nanoparticle slurry flows into the operating valve gap of high pressure homogenizer by feed inlet, stitches in operating valve
It is extruded in gap.The squeeze pressure in operating valve gap needs to pass through at this time due to that can be generated variation by interparticle mutual extrusion
It manually adjusts, the work pressure of the high pressure homogenizer of the squeeze pressure and earlier set that are subject to nanoparticle between operating valve gap
Power is consistent, so that nano particle diameter can uniformly reduce.
Very low pressure will be born after nanoparticle slurry passes through operating valve gap, which is generally 1bar, institute
Void effect can be generated with the nanoparticle slurry of instantaneous loss of pressure, so that nanoparticle slurry has very fast speed to eject
Come, with the stronger impact force of this output.Nanoparticle slurry can generate between nanoparticle simultaneously during high speed is sprayed
Certain shearing force, the shearing force reduce nano particle diameter, are uniformly dispersed in water.
In one embodiment, the second predetermined time was 30min-60min.
Specifically, the high-pressure homogeneous time is 30min-60min, which can realize nanoparticle shear history for the first time；It is excellent
Choosing, the second preset time is 30min.
In step S26, the discharge port of high pressure homogenizer flows out the nanoparticle slurry after being sheared, by the nanometer after shearing
It after particle slurry is collected together, also needs that high pressure homogenizer is washed with deionized, it is dry that the discharge port to high pressure homogenizer goes out liquid
Until net free from admixture, high pressure homogenizer switch is closed, the rotor speed of high pressure homogenizer is adjusted to 0.
In one embodiment, step S2 is executed 3-6 times.
Specifically, nano particle diameter can be controlled by the pressure and shear time for adjusting high pressure homogenizer, simultaneously
It is also related to number of processes.Nanoparticle slurry number of processing in high pressure homogenizer is more, the nanoparticle seed after shearing
Diameter is smaller, and nanoparticle slurry number of processing in high pressure homogenizer is fewer, and the nano particle diameter after shearing is bigger.This reality
It applies in example, preferred nanoparticle slurry number of processing in high pressure homogenizer is 3-6 times.
Fig. 3 is the flow chart of the step S3 of preparation method provided by the invention.
In one embodiment, step S3 includes:
S31: opening Microfluidizer switch, and the operating pressure for adjusting Microfluidizer is 1500bar-1800bar.
S32: the homogeneous chamber of Microfluidizer is added by feed inlet for the nanoparticle slurry that step S2 is sheared
In.
S33: nanoparticle slurry carries out secondary shearing in the homogeneous chamber of Microfluidizer, in Microfluidizer work
After reaching the third predetermined time as the time, the nanoparticle aqueous dispersions of obtained stable dispersion are exported, and close microjet
Homogenizer.
Specifically, in step S32, Microfluidizer switch is opened, the pressure adjustment knob of Microfluidizer is passed through
The operating pressure for adjusting Microfluidizer is 1500bar-1800bar.Under the pressure limit, nano particle diameter can be made
Reduce within the short period；Preferably, the operating pressure of Microfluidizer is 1700bar.
In step S31, the valve between feed inlet and high pressure homogenizer is to close at this time, will be collected into step S26
Nanoparticle slurry by feed inlet be added Microfluidizer homogeneous chamber in.
In step S33, Microfluidizer is mainly made of homogeneous chamber and booster body, and the intracavitary portion of homogeneous is set as
" Z " type channel, under the action of booster body, the nanoparticle slurry under high pressure conditions rapidly passes through homogeneous chamber, opposite
Jet stream under direction, and carry out high velocity impact.Nanoparticle slurry is in this process by shearing force, the higher-order of oscillation, hole effect
It should be acted on knock-on effect, to realize the secondary shearing and crushing to nanoparticle slurry.
The product of discharge port outflow of Microfluidizer is collected up to the nanoparticle aqueous dispersions of stable dispersion, this is received
Nano-particles size in rice corpuscles aqueous dispersions is 50-300nm, and nanoparticle aqueous dispersions can be stablized placement one month or more
Do not occur reunion sedimentation phenomenon.
In one embodiment, the third predetermined time is 30min-60min.
Specifically, microjet homogenizing time is 30min-60min, which can realize the effective of nano particle diameter
It reduces；Preferably, the third predetermined time is 60min.
In one embodiment, step S3 is executed 3-6 times.
Specifically, nano particle diameter can be controlled by the pressure and shear time for adjusting Microfluidizer, together
When it is also related to number of processes.Nanoparticle slurry number of processing in Microfluidizer is more, the nanoparticle after shearing
Seed diameter is smaller, and nanoparticle slurry number of processing in Microfluidizer is fewer, and the nano particle diameter after shearing is got over
Greatly.In the present embodiment, preferred nanoparticle slurry number of processing in Microfluidizer is 3-6 times.
In one embodiment, the homogeneous chamber of Microfluidizer is made of diamond.
Specifically, diamond material is harder, can be avoided the equipment in particle encounter and cracks, falls the situations such as bits, with
Avoid pollution product.Diamond is lower than the cost of natural diamond simultaneously, more economical.
Embodiment one:
Step 1: graphene nano particle and water being mixed, mass ratio 1:5；By mixed graphene nano particle and
Water carries out mechanical stirring, is made into graphene nano particle slurry, and wherein speed of agitator is 400 rpms, and mixing time is
60min。
Step 2: graphene nano particle slurry being sheared: first closing Microfluidizer switch, then opens high pressure
Homogenizer switch；Feed inlet is added；Adjusting high pressure homogenizer rotor speed is 450 rpms；Adjust the work of high pressure homogenizer
Making pressure is 1500bar；The high-pressure homogeneous time is 30min.
Step 3: step 2 is repeated 3 times.
Step 4: the pretreated graphene nano particle slurry of step 3 being collected together, height is washed with deionized
Homogenizer is pressed, until going out the clean free from admixture of liquid to discharge port, high pressure homogenizer switch is closed, rotor speed is adjusted to 0.
Step 5: graphene nano particle slurry being subjected to secondary shearing: opening Microfluidizer switch；It will be in step 4
Feed inlet is added in the graphene nano particle slurry being collected into；The operating pressure for adjusting Microfluidizer is 1600bar；It is micro- to penetrate
Stream homogenizing time is 60min.
Step 6: step 5 is repeated 3 times.
Step 7: treated the product of collection step 6 to get stable dispersion graphene nano particle water dispersion liquid, with swashing
Light particle size instrument nano particle diameter range is 120-280nm, can stablize and place January without precipitating.
Embodiment two:
Step 1: graphene nano particle and water being mixed, mass ratio 1:5；By mixed graphene nano particle and
Water carries out mechanical stirring, is made into graphene nano particle slurry, and wherein speed of agitator is 400 rpms, and mixing time is
60min。
Step 2: graphene nano particle slurry being sheared: first closing Microfluidizer switch, then opens high pressure
Homogenizer switch；Feed inlet is added；Adjusting high pressure homogenizer rotor speed is 450 rpms；Adjust the work of high pressure homogenizer
Making pressure is 1500bar；The high-pressure homogeneous time is 30min.
Step 3: step 2 is repeated 4 times.
Step 4: the pretreated graphene nano particle slurry of step 3 is collected together；Height is washed with deionized
Homogenizer is pressed, until going out the clean free from admixture of liquid to discharge port, high pressure homogenizer switch is closed, rotor speed is adjusted to 0.
Step 5: graphene nano particle slurry being subjected to secondary shearing: opening Microfluidizer switch；It will be in step 4
Feed inlet is added in the graphene nano particle slurry being collected into；The operating pressure for adjusting Microfluidizer is 1600bar；It is micro- to penetrate
Stream homogenizing time is 60min.
Step 6: step 5 is repeated 4 times.
Step 7: product uses laser to get the graphene nano particle water dispersion liquid of stable dispersion after the processing of collection step 6
Particle size instrument nano particle diameter range is 80-200nm, can stablize storage one week without precipitating.
Embodiment three:
Step 1: graphene nano particle and water being mixed, mass ratio 1:5；By mixed graphene nano particle and
Water carries out mechanical stirring, is made into graphene nano particle slurry, and wherein speed of agitator is 400 rpms, and mixing time is
60min。
Step 2: graphene nano particle slurry being sheared: first closing Microfluidizer switch, then opens high pressure
Homogenizer switch；Feed inlet is added；Adjusting high pressure homogenizer rotor speed is 450 rpms；Adjust the work of high pressure homogenizer
Making pressure is 1500bar；The high-pressure homogeneous time is 30min.
Step 3: step 2 is repeated 6 times.
Step 4: the pretreated graphene nano particle slurry of step 3 is collected together；Height is washed with deionized
Homogenizer is pressed, until going out the clean free from admixture of liquid to discharge port, high pressure homogenizer switch is closed, rotor speed is adjusted to 0.
Step 5: graphene nano particle slurry being subjected to secondary shearing: opening Microfluidizer switch；It will be in step 4
Feed inlet is added in the graphene nano particle slurry being collected into；Adjusting knob adjust Microfluidizer operating pressure be
1600bar；Microjet homogenizing time is 60min.
Step 6: step 5 is repeated 6 times.
Step 7: product uses laser to get the graphene nano particle water dispersion liquid of stable dispersion after the processing of collection step 6
Particle size instrument nano particle diameter range is 50-160nm, stablizes storage one week without precipitating.
Example IV:
Step 1: graphene nano particle and water being mixed, mass ratio 2:8；By mixed graphene nano particle and
Water carries out mechanical stirring, is made into graphene nano particle slurry, and wherein speed of agitator is 400 rpms, and mixing time is
60min。
Step 2: graphene nano particle slurry being sheared: first closing Microfluidizer switch, then opens high pressure
Homogenizer switch；Feed inlet is added；Adjusting high pressure homogenizer rotor speed is 450 rpms；Adjust the work of high pressure homogenizer
Making pressure is 1600bar；The high-pressure homogeneous time is 30min.
Step 3: step 2 is repeated 4 times.
Step 4: the pretreated graphene nano particle slurry of step 3 is collected together；Height is washed with deionized
Homogenizer is pressed, until going out the clean free from admixture of liquid to discharge port, high pressure homogenizer switch is closed, rotor speed is adjusted to 0.
Step 5: graphene nano particle slurry being subjected to secondary shearing: opening Microfluidizer switch；It will be in step 4
Feed inlet is added in the graphene nano particle slurry being collected into；Adjusting knob adjust Microfluidizer operating pressure be
1700bar；Microjet homogenizing time is 30min.
Step 6: step 5 is repeated 6 times.
Step 7: product uses laser to get the graphene nano particle water dispersion liquid of stable dispersion after the processing of collection step 6
Particle size instrument nano particle diameter range is 80-270nm, stablizes storage one week without precipitating.
Embodiment five:
Step 1: graphene nano particle and water being mixed, mass ratio 2:8；By mixed graphene nano particle and
Water carries out mechanical stirring, is made into graphene nano particle slurry, and wherein speed of agitator is 400 rpms, and mixing time is
60min。
Step 2: graphene nano particle slurry being sheared: first closing Microfluidizer switch, then opens high pressure
Homogenizer switch；Feed inlet is added；Adjusting high pressure homogenizer rotor speed is 450 rpms；Adjust the work of high pressure homogenizer
Making pressure is 1600bar；The high-pressure homogeneous time is 60min.
Step 3: step 2 is repeated 4 times.
Step 4: the pretreated graphene nano particle slurry of step 3 is collected together；Height is washed with deionized
Homogenizer is pressed, until going out the clean free from admixture of liquid to discharge port, high pressure homogenizer switch is closed, rotor speed is adjusted to 0.
Step 5: graphene nano particle slurry being subjected to secondary shearing: opening Microfluidizer switch；It will be in step 4
Feed inlet is added in the graphene nano particle slurry being collected into；Adjusting knob adjust Microfluidizer operating pressure be
1700bar；Microjet homogenizing time is 60min.
Step 6: step 5 is repeated 6 times.
Step 7: product uses laser to get the graphene nano particle water dispersion liquid of stable dispersion after the processing of collection step 6
Particle size instrument nano particle diameter range are as follows: 50-140nm stablizes storage one week without precipitating.
The present invention is directed to protect a kind of preparation method of nanoparticle aqueous dispersions, comprising the following steps: by raw material nano
After particle is mixed with water by preset quality proportion, mechanical stirring is carried out in preset rotation speed and the first preset time, obtains nanometer
Particle slurry；Nanoparticle slurry addition high pressure homogenizer is sheared again, to reduce nanoparticle in nanoparticle slurry
Partial size；Microfluidizer finally is added in the nanoparticle slurry after shearing and carries out secondary shearing, obtains nanoparticle moisture
Dispersion liquid, wherein the partial size of nanoparticle is 50-300nm in nanoparticle aqueous dispersions.It is penetrated by high pressure homogenizer shearing with micro-
Stream homogenizer secondary shearing carries out preparing nanoparticle aqueous dispersions, and preparation process is penetrated by adjusting high pressure homogenizer shearing with micro-
Pressure and the processing time for flowing homogenizer, it can control the size of nanoparticle, so that the nanoparticle aqueous dispersions of preparation are stablized
Property it is good, placement one month or more can be stablized.Method is simple, does not need using organic solvent and stabilizer, it is dirty that there is no environment
Dye and subsequent liquid waste processing problem provide one simply for the preparation of nanoparticle stable dispersions, and efficient method is easy to
It is a wide range of to promote.
It should be understood that above-mentioned specific embodiment of the invention is used only for exemplary illustration or explains of the invention
Principle, but not to limit the present invention.Therefore, that is done without departing from the spirit and scope of the present invention is any
Modification, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.In addition, appended claims purport of the present invention
Covering the whole variations fallen into attached claim scope and boundary or this range and the equivalent form on boundary and is repairing
Change example.
Claims (10)
1. a kind of preparation method of nanoparticle aqueous dispersions characterized by comprising
S1: it after raw material nano particle is mixed with water by preset quality proportion, is carried out in preset rotation speed and the first preset time
Mechanical stirring obtains nanoparticle slurry；
S2: nanoparticle slurry addition high pressure homogenizer is sheared, to reduce nanometer in the nanoparticle slurry
Particle diameter；
S3: Microfluidizer is added in the nanoparticle slurry after shearing and carries out secondary shearing, obtains nanoparticle water
Dispersion liquid, wherein the partial size of nanoparticle is 50-300nm in nanoparticle aqueous dispersions.
2. preparation method according to claim 1, which is characterized in that
Step S2 is executed 3-6 times.
3. preparation method according to claim 1 or 2, which is characterized in that
Step S3 is executed 3-6 times.
4. preparation method according to claim 1, which is characterized in that
The preset quality proportion is 1-2:5-10.
5. preparation method according to claim 1, which is characterized in that
The preset rotation speed is 300rpm-500rpm；
First preset time is 30min-60min.
6. preparation method according to claim 1 or 2, which is characterized in that the step S2 includes:
S21: closing the Microfluidizer, opens the high pressure homogenizer；
S22: the nanoparticle slurry is added in the high pressure homogenizer by feed inlet；
S23: adjust the high pressure homogenizer revolving speed be 400rpm-500rpm, make the high pressure homogenizer under the revolving speed into
Row preheating；
S24: the operating pressure of the high pressure homogenizer is set as 1500bar-1800bar；
S25: the nanoparticle slurry is squeezed from the operating valve gap that the feed inlet flows into the high pressure homogenizer,
The squeeze pressure between the operating valve gap is adjusted, the operating pressure of itself and the high pressure homogenizer is consistent；
S26: after the working time of the high pressure homogenizer reached for the second predetermined time, the discharging of the high pressure homogenizer is collected
The nanoparticle slurry of mouth outflow, closes the high pressure homogenizer.
7. preparation method according to claim 6, which is characterized in that
Second preset time is 30min-60min.
8. preparation method according to claim 1, which is characterized in that the step S3 includes:
S31: opening the Microfluidizer switch, and the operating pressure for adjusting the Microfluidizer is 1500bar-
1800bar；
S32: the equal of the Microfluidizer is added by feed inlet in the nanoparticle slurry that step S2 is sheared
In matter chamber；
S33: the nanoparticle slurry carries out secondary shearing in the homogeneous chamber of the Microfluidizer, in the microjet
After the homogenizer working time reaches the third predetermined time, the nanoparticle aqueous dispersions of obtained stable dispersion are exported, and closes
Close the Microfluidizer.
9. preparation method according to claim 8, which is characterized in that
The third predetermined time is 30min-60min.
10. preparation method according to claim 1 or 8, which is characterized in that
The homogeneous chamber of the Microfluidizer is made of diamond.
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| CN116510548A (en) * | 2023-07-04 | 2023-08-01 | 浙江汉信科技有限公司 | Slurry stirring method and stirring device |
| CN116510549A (en) * | 2023-07-04 | 2023-08-01 | 浙江汉信科技有限公司 | Stirring method and device suitable for high-capacity and high-viscosity slurry |
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