CN103920434B - A kind of particle diameter and morphology controllable there is carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of electric charge and optics opposite sex feature and preparation method thereof - Google Patents
A kind of particle diameter and morphology controllable there is carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of electric charge and optics opposite sex feature and preparation method thereof Download PDFInfo
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Abstract
What the invention discloses a kind of particle diameter and morphology controllable has carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of electric charge and optics opposite sex feature and preparation method thereof, it is characterized in that: by adding carbon black in decentralized photo solution, and control the viscosity of collecting liquid, obtain and form carbon black/polytetrafluoroethylene (PTFE) Janus microballoon by two polytetrafluoroethylene (PTFE) hemisphere, and wherein in a polytetrafluoroethylene (PTFE) hemisphere containing carbon black, polytetrafluoroethylene (PTFE) hemisphere containing carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black is white.Carbon black/polytetrafluoroethylene (PTFE) Janus the microballoon with electric charge and optics opposite sex feature prepared by the present invention is obvious with the line of demarcation not containing the polytetrafluoroethylene (PTFE) hemisphere of carbon black containing the polytetrafluoroethylene (PTFE) hemisphere of carbon black, sphericity is better, polytetrafluoroethylmaterial material can resist adverse circumstances, and water and oil can not be glued, difficult and chemical reagent reacts, and stability is better.
Description
Technical field
The invention belongs to the preparation field of Janus microballoon, be specifically related to carbon black/polytetrafluoroethylene (PTFE) Janus microballoon and preparation method thereof.Background technology
In recent years, the research for anisotropic Janus microballoon becomes study hotspot gradually.The title of Janus is proposed in the Nobel Prize award-giving meeting of 1991 by DeGennes the earliest, derives from the name of a two-sided god in ancient Roman's mythology, and being used for stating surperficial two hemispheres mask has particle of different nature.Because its two sides has different character, therefore its application prospect widely, relates to physics, chemistry, biological, the fields such as material.
Wherein there is electric charge and optically anisotropic microballoon due to the unique texture of himself, be more and more subject to people's attention.As the Electronic Paper for showing field, under extra electric field, realizing the upset of the different particle of both sides color by changing direction of an electric field, reaching the principle of colour developing.
The people such as DaisukeSuzuki, by golden sputtering method, by gold on local complexity on polystyrene microsphere, carry out the electric charge opposite sex Janus microballoon of synthesized semiconductor semi-insulator.But the line of demarcation on its both sides of method of this splash is not very clear, and the distribution being difficult to guarantee fund is more even.
And can the micro-fluidic technologies of control accurate Microsphere Size be subject to people's attention equally.The double capillary microfluid adopting microfluidic channel to flow method and Shin-HyunKim altogether as TakasiNisisako flows altogether with full-bodied two kinds of fluids and cuts into drop and realizes Janus microballoon.This method needs guarantee two kinds of liquid dissolved each other can not spread when parallel flowing, is therefore comparatively difficult to regulate.
Obtain size can from tens microns to the regulation and control of hundreds of micron, interface is clear, corrosion-resistant and the microballoon with electric charge and the optics opposite sex is the direction that scientists is made great efforts always.
Summary of the invention
In order to solve the problem, the object of the present invention is to provide and to be a kind ofly made up of two corrosion resistant polytetrafluoroethylene (PTFE) hemisphere and the preparation method with electric charge and the images generated carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of optics of particle diameter wherein containing carbon black in a polytetrafluoroethylene (PTFE) hemisphere and morphology controllable.
Another object of the present invention is to provide the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of a kind of particle diameter and morphology controllable.
Technical solution problem of the present invention, adopts following technical scheme:
The preparation method with the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of electric charge and optics opposite sex feature of particle diameter of the present invention and morphology controllable, its feature is to carry out as follows:
A, preparation decentralized photo solution: carbon black is added in distilled water, make carbon black dispersion even by ball milling, obtain mixed liquor; In described mixed liquor, add ptfe emulsion, by vibration, ptfe emulsion is mixed with described mixed liquor, then leave standstill to bubble collapse, obtain dispersion and to mix liquid; Solution surface can be made after vibration to produce bubble, should leave standstill to bubble collapse and re-use, because bubble can affect the size uniformity of gained dispersed phase drop.
In described carbon black, distilled water and ptfe emulsion, the mass ratio of polytetrafluoroethylene (PTFE) is: 0.03 ~ 0.2:7:3.5;
Liquid is collected in b, preparation: 1:0.1 ~ 5 in mass ratio, mix dimethicone with silicone oil thickener, stir and leave standstill to bubble collapse, obtaining collection liquid;
C, preparation continuous phase solution: using dimethicone as continuous phase solution;
D, decentralized photo solution and continuous phase solution are passed into microfluidic device, the flow controlling decentralized photo solution and continuous phase solution is respectively 1 ~ 10ul/min and 50 ~ 200ul/min;
E, outflow port place at decentralized photo solution, decentralized photo solution is constantly sheared by continuous phase solution, forms the dispersed dispersed phase drop having carbon black;
F, to be collected by described dispersed phase drop in collection liquid that step b prepares, and evaporate the moisture in described dispersed phase drop by high temperature drying, while making carbon black gather the side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon; Because the moisture in drop slowly evaporates, it is made finally to become microspheres with solid.In this section of process, carbon black can gather side wherein gradually simultaneously.Because silicon oil viscosity is very large, the sedimentation of drop can slowly, and had cured before it is deposited to bottom, therefore sphericity is better.
G, by the pending Janus microballoon of step f gained from collection liquid take out, carry out washing by soaking with benzinum, remove the silicone oil of described pending Janus microsphere surface, and then wash away the benzinum of pending Janus microsphere surface with ethanol, dry under room temperature, obtain and treat calcining Janus microballoon; Preferably, the number of times of silicone oil is cleaned more than 4 times, to ensure to remove silicone oil completely with benzinum; With the number of times of ethanol purge benzinum more than 2 times, to ensure to remove benzinum completely.
H, treat that calcining Janus microballoon carries out high-temperature calcination by described, obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and the different in nature feature of optics of size uniformity.
Preparation method of the present invention, its feature is also: by regulating and controlling the flow of decentralized photo solution and continuous phase solution, regulate and control the particle diameter of described dispersed phase drop, thus the particle diameter of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon, obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of size tunable.
By the mass concentration of carbon black in regulation and control decentralized photo solution, regulate and control the pattern of described dispersed phase drop, thus the pattern of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon, obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of morphology controllable.
Preferably, the viscosity of described collection liquid is not less than 100,000 centipoises.Collecting the too low meeting of viscosity of liquid causes water-drop sedimentation velocity too fast, makes drop just sink to container bottom before being cured, and makes the bottom of ball occur one piece of flat region.The higher ball sinking speed that can make of viscosity is slack-off, and just have cured before conceding points bottom sinking to, the sphericity obtained is better.
Preferably, in step f, the condition of high temperature drying is: temperature 90 DEG C, 24 ~ 36 hours time.
Preferably, the condition of the high-temperature calcination in step h is 200 ~ 350 DEG C, 2 ~ 4 hours.Temperature is higher than 400 DEG C, and polytetrafluoroethylene (PTFE) can decompose.
Invention further provides the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature obtained by above-mentioned preparation method, its feature is: described microballoon is made up of two polytetrafluoroethylene (PTFE) hemisphere, and wherein in a polytetrafluoroethylene (PTFE) hemisphere containing carbon black.Polytetrafluoroethylene (PTFE) hemisphere containing carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black is white.
What preparation method of the present invention obtained has the carbon black/polytetrafluoroethylene (PTFE) Janus microspherulite diameter of electric charge and optics opposite sex feature between 100 ~ 700 microns, and CV is less than 3%.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the polytetrafluoroethylene (PTFE) hemisphere had containing carbon black in the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of electric charge and optics opposite sex feature prepared by the present invention is obvious with the line of demarcation not containing the polytetrafluoroethylene (PTFE) hemisphere of carbon black, sphericity is better, polytetrafluoroethylmaterial material can resist adverse circumstances, and water and oil can not be glued, difficult and chemical reagent reacts, and stability is better;
2, the carbon black prepared by the present invention/polytetrafluoroethylene (PTFE) Janus microballoon due to two hemisphere be all polytetrafluoroethylene (PTFE) material, interhemispheric adhesion is very tight, is difficult to disconnect;
3, the present invention is by regulating the speed of decentralized photo and continuous phase, the mono-dispersion microballoon of different size can be obtained, microballoon size can reach tens to hundreds of micron, has widened electric charge-optical anisotropy microballoon and has twisted the application of ball in electric ink field as double-colored;
4, the method for carbon black/polytetrafluoroethylene (PTFE) Janus microballoon prepared of the present invention, by the mass concentration of carbon black in regulation and control decentralized photo solution, carbon black/polytetrafluoroethylene (PTFE) Janus the microballoon of morphology controllable can be obtained, the resolution adjustment of Electronic Paper can be used for containing the ratio shared by carbon black region according to the later stage.
Accompanying drawing explanation
Fig. 1 is the present invention's microfluidic control device used schematic diagram;
Fig. 2 is the enlarged drawing of microfluidic device part A of the present invention;
Fig. 3 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon prepared by embodiment 1;
Fig. 4 is the picture that the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of embodiment 1 preparation overturns under the electric field;
Fig. 5 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon prepared by embodiment 2;
Fig. 6 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon prepared by embodiment 3;
Fig. 7 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon prepared by embodiment 4;
Fig. 8 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon prepared by embodiment 4;
Number in the figure: 1-decentralized photo syringe pump; 2-decentralized photo syringe; 3-continuous phase syringe pump; 4-continuous phase syringe; 5-decentralized photo flexible pipe; 6-continuous phase flexible pipe; The threeway of 7-T type; 8-outer catheter; 9-returnable; 10-collects liquid; 11-capillary; 12-dispersed phase drop; 13-bilateral; 14-connecting hose.
Specific embodiment
First the microfluidic control device that embodiments of the invention adopt is introduced.
As shown in Figure 1 and Figure 2, microfluidic control device comprises the continuous phase syringe 4 be arranged on continuous phase syringe pump 3, the decentralized photo syringe 2 be arranged on decentralized photo syringe pump 1, T-shaped threeway 7 and returnable 9;
Continuous phase syringe 4 is connected by first port of continuous phase flexible pipe 6 with T-shaped threeway 7;
Second port of T-shaped threeway 7 is communicated with outer catheter 8;
3rd port of T-shaped threeway and the second port are on the same line; The outflow port being arranged on the capillary 11 in T-shaped threeway is inserted in outer catheter 8 through the second port, and flow into port and be connected with the outflow port of decentralized photo flexible pipe 5 through the 3rd port, the inflow port of decentralized photo flexible pipe 5 is communicated with decentralized photo syringe 2; The output port of outer catheter is provided with returnable 9.
Concrete, capillary 11 is communicated with by bilateral 13 with decentralized photo flexible pipe 5, and capillary 11 is fixed by connecting hose 14 with outer catheter 8.
Polyfluortetraethylene pipe selected by output duct and continuous phase conduit; Decentralized photo flexible pipe 5 and continuous phase flexible pipe 6 are of a size of external diameter 1590um, internal diameter 762um; Capillary 11 external diameter is 358um, and internal diameter is 252um.
During use, decentralized photo solution and continuous phase solution are respectively charged into decentralized photo syringe 2 and continuous phase syringe 4, collection liquid 10 is loaded returnable 9, start microfluidic control device, control the fltting speed of continuous phase syringe pump 3 and decentralized photo syringe pump 1, decentralized photo solution through capillary, at outflow port (i.e. the outflow port of the decentralized photo solution) place of capillary 11, constantly sheared by continuous phase solution, form the dispersed dispersed phase drop 12 having carbon black; Dispersed phase drop 12 is collected in the collection liquid 10 in returnable 9,
Then returnable is put into drying box, along with the evaporation of moisture, drop is solid-state-microspherical by liquid conversion gradually.Concentrate solidification process along with drop, the carbon black be dispersed in dispersed phase drop gathers the side of drop gradually and finally forms the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon be made up of with the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black of white the polytetrafluoroethylene (PTFE) hemisphere containing carbon black of black originally.Its preparation principle is: carbon black fine particle is dispersed in ptfe emulsion, and in microfluidic control device, form the equally distributed ptfe emulsion drop of carbon black.Along with the moisture evaporation in drop solidification process, ion concentration in emulsion improves constantly, the zeta potential of carbon black micelle is caused to reduce gradually, carbon black fine particle is finally made to assemble, and now polytetrafluoroethylene (PTFE) still Absorbable organic halogens be dispersed in system, form side until last containing carbon black, opposite side is not containing the polytetrafluoroethylene (PTFE) microballoon with Janus structure of carbon black.
Decentralized photo solution is flowed into the capillary in threeway under the promotion of syringe pump by conduit, be subject to forming the identical drop of size one by one from the shearing force of continuous phase at the port of capillary, in the container flow into for collecting through outer catheter along with continuous phase.Due to
d
dropand d
capillaryrefer to the diameter of drop and capillary, μ
continuous phaseand μ
decentralized photorefer to the viscosity of continuous phase and decentralized photo, V
continuous phaseand V
decentralized photorefer to the speed of continuous phase and decentralized photo, K is coefficient.By regulating the size of capillary, and the viscosity of continuous phase and decentralized photo and speed, we can obtain the drop of different size.
Below in conjunction with specific embodiment, set forth related content of the present invention further.It is to be noted, these embodiments are only not used in for illustration of the present invention and limit the scope of the invention, and, after having read content of the present invention, relevant technical staff in the field can make various change or amendment to the present invention, and these equivalent form of values fall into the application's appended claims limited range equally.
Embodiment 1
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature as follows:
A, preparation decentralized photo solution: 0.1g carbon black is added in 7g distilled water, within 4 hours, make carbon black dispersion even by planetary ball mill ball milling (revolution speed is 200rpm), obtain mixed liquor; In mixed liquor, add 7g ptfe emulsion (polytetrafluoroethylene (PTFE) concentration is 50%), by supersonic oscillations (frequency 53KHz, 20 minutes), ptfe emulsion is mixed with mixed liquor, then leave standstill to bubble collapse, obtain dispersion and to mix liquid;
Liquid is collected in b, preparation: be that the dimethicone of 500 centipoises mixes with 40g thickener (thunder nation chemical industry RB-1200 dimethicone 1,000,000 cs) by 40g viscosity, stir and leave standstill to bubble collapse, obtaining collection liquid, and the viscosity of collection liquid is 100,000 centipoises.
C, preparation continuous phase solution: be that the dimethicone of 500 centipoises is as continuous phase solution using viscosity;
D, 1ml decentralized photo syringe pump decentralized photo solution and continuous phase solution being respectively charged into microfluidic control device and 20ml continuous phase syringe pump, liquid will be collected and load returnable, the flow controlling decentralized photo solution and continuous phase solution is respectively 1ul/min and 50ul/min, and capillary size is internal diameter 252um, external diameter 358um; Decentralized photo flexible pipe 5 and continuous phase flexible pipe 6 are of a size of external diameter 1590um, internal diameter 762um; Outer catheter for deriving drop is of a size of internal diameter 1.6mm, external diameter 3.2mm;
E, starting drive, at the outflow port place of decentralized photo solution, decentralized photo solution is constantly sheared by continuous phase solution, forms the dispersed dispersed phase drop having carbon black;
F, collect dispersed phase drop in returnable collection liquid, and by the moisture in high temperature drying (90 DEG C, 24 hours) evaporation dispersed phase drop, while making carbon black gather the side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, by the pending Janus microballoon of step f gained from collection liquid take out, washing by soaking is carried out with benzinum in vent cabinet, remove the silicone oil of pending Janus microsphere surface, and then the benzinum of pending Janus microsphere surface is washed away with ethanol, dry under room temperature, obtain and treat calcining Janus microballoon; The number of times cleaning silicone oil with benzinum is 4 times, to ensure to remove silicone oil completely; It is 2 times with the number of times of ethanol purge benzinum, to ensure to remove benzinum completely.
H, will treat that calcining Janus microballoon carries out high-temperature calcination (300 DEG C, 2 hours), obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and the different in nature feature of optics of size uniformity.
Fig. 3 is the optical microscope picture of thus obtained microsphere, and can find out that microballoon is made up of two hemisphere, the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black is white.Microspherulite diameter is homogeneous, has monodispersity, and particle diameter is 640um.
The present half of optics metamer of thus obtained microsphere is black, and half is white.
Electric charge metamer is now as follows: containing carbon black hemisphere and not containing the hemisphere of carbon black in external electric field owing to having different electrical properties, therefore can produce electric dipole, be placed on by microballoon between two electrode plate, add voltage 100V, ball overturns, as shown in Figure 4.
Embodiment 2
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature as follows:
A, preparation decentralized photo solution: 0.1g carbon black is added in 7g distilled water, within 4 hours, make carbon black dispersion even by planetary ball mill ball milling (revolution speed is 200rpm), obtain mixed liquor; 7g ptfe emulsion (polytetrafluoroethylene (PTFE) concentration is 50%) is added in described mixed liquor, by supersonic oscillations (frequency 53KHz, 20 minutes) ptfe emulsion is mixed with described mixed liquor, then leave standstill to bubble collapse, obtain dispersion and to mix liquid;
Liquid is collected in b, preparation: be that the dimethicone of 500 centipoises mixes with 40g thickener (thunder nation chemical industry RB-1200 dimethicone 1,000,000 cs) by 40g viscosity, stir and leave standstill to bubble collapse, obtaining collection liquid, viscosity 100,000 centipoise of collection liquid.
C, preparation continuous phase solution: be that the dimethicone of 500 centipoises is as continuous phase solution using viscosity;
D, 1ml decentralized photo syringe pump decentralized photo solution and continuous phase solution being respectively charged into microfluidic control device and 20ml continuous phase syringe pump, liquid will be collected and load returnable, the flow controlling decentralized photo solution and continuous phase solution is respectively 1ul/min and 100ul/min, and capillary size is internal diameter 252um, external diameter 358um; Decentralized photo flexible pipe 5 and continuous phase flexible pipe 6 are of a size of external diameter 1590um, internal diameter 762um; Outer catheter for deriving drop is of a size of internal diameter 1.6mm, external diameter 3.2mm;
E, starting drive, at the outflow port place of decentralized photo solution, decentralized photo solution is constantly sheared by continuous phase solution, forms the dispersed dispersed phase drop having carbon black;
F, collect described dispersed phase drop in returnable collection liquid, and the moisture evaporated by high temperature drying (90 DEG C, 24 hours) in described dispersed phase drop, while making carbon black gather the side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, by the pending Janus microballoon of step f gained from collection liquid take out, washing by soaking is carried out with benzinum in vent cabinet, remove the silicone oil of described pending Janus microsphere surface, and then the benzinum of pending Janus microsphere surface is washed away with ethanol, dry under room temperature, obtain and treat calcining Janus microballoon; The number of times cleaning silicone oil with benzinum is 4 times, to ensure to remove silicone oil completely; It is 2 times with the number of times of ethanol purge benzinum, to ensure to remove benzinum completely.
H, will treat that calcining Janus microballoon carries out high-temperature calcination (300 DEG C, 2 hours), obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and the different in nature feature of optics of size uniformity.
Fig. 5 is the optical microscope picture of thus obtained microsphere, and can find out that microballoon is made up of two hemisphere, the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black is white.Microspherulite diameter is homogeneous, has monodispersity, and particle diameter is 470um.
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature by the mode identical with embodiment 1, difference is: the flow of continuous phase solution becomes and is increased to 100ul/min by 50ul/min, and the diameter of microballoon is reduced to 470um from 640um.Can see, increase the flow of continuous phase, the microsphere diameter of gained reduces.Therefore the regulation and control of particle diameter can be realized by adjustment continuous phase flow.
Embodiment 3
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature as follows:
A, preparation decentralized photo solution: 0.1g carbon black is added in 7g distilled water, within 4 hours, make carbon black dispersion even by planetary ball mill ball milling (revolution speed is 200rpm), obtain mixed liquor; In mixed liquor, add 7g ptfe emulsion (polytetrafluoroethylene (PTFE) concentration is 50%), by supersonic oscillations (frequency 53KHz, 20 minutes), ptfe emulsion is mixed with mixed liquor, then leave standstill to bubble collapse, obtain dispersion and to mix liquid;
Liquid is collected in b, preparation: be that the dimethicone of 500 centipoises mixes with 40g thickener (thunder nation chemical industry RB-1200 dimethicone 1,000,000 cs) by 40g viscosity, stir and leave standstill to bubble collapse, obtaining collection liquid, viscosity 100,000 centipoise of collection liquid.
C, preparation continuous phase solution: be that the dimethicone of 500 centipoises is as continuous phase solution using viscosity;
D, 1ml decentralized photo syringe pump decentralized photo solution and continuous phase solution being respectively charged into microfluidic control device and 20ml continuous phase syringe pump, liquid will be collected and load returnable, the flow controlling decentralized photo solution and continuous phase solution is respectively 1ul/min and 150ul/min, and capillary size is internal diameter 252um, external diameter 358um; Decentralized photo flexible pipe 5 and continuous phase flexible pipe 6 are of a size of external diameter 1590um, internal diameter 762um; Outer catheter for deriving drop is of a size of internal diameter 1.6mm, external diameter 3.2mm;
E, starting drive, at the outflow port place of decentralized photo solution, decentralized photo solution is constantly sheared by continuous phase solution, forms the dispersed dispersed phase drop having carbon black;
F, collect dispersed phase drop in returnable collection liquid, and the moisture evaporated by high temperature drying (90 DEG C, 24 hours) in described dispersed phase drop, while making carbon black gather the side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, by the pending Janus microballoon of step f gained from collection liquid take out, washing by soaking is carried out with benzinum in vent cabinet, remove the silicone oil of described pending Janus microsphere surface, and then the benzinum of pending Janus microsphere surface is washed away with ethanol, dry under room temperature, obtain and treat calcining Janus microballoon; The number of times cleaning silicone oil with benzinum is 4 times, to ensure to remove silicone oil completely; It is 2 times with the number of times of ethanol purge benzinum, to ensure to remove benzinum completely.
H, will treat that calcining Janus microballoon carries out high-temperature calcination (300 DEG C, 2 hours), obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and the different in nature feature of optics of size uniformity.
Fig. 6 is the optical microscope picture of thus obtained microsphere, and can find out that microballoon is made up of two hemisphere, the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black is white.Microspherulite diameter is homogeneous, has monodispersity, and particle diameter is 107um.
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature by the mode identical with embodiment 2, difference is: the flow of continuous phase solution becomes and is increased to 150ul/min by 100ul/min, and the diameter of microballoon is reduced to 107um from 470um.Can see, continue the flow increasing continuous phase, the microsphere diameter of gained still reduces.Therefore, embodiment 1,2,3 contrasts the known regulation and control that can be realized particle diameter by adjustment continuous phase flow.
Embodiment 4
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature as follows:
A, preparation decentralized photo solution: 0.03g carbon black is added in 7g distilled water, within 4 hours, make carbon black dispersion even by planetary ball mill ball milling (revolution speed is 200rpm), obtain mixed liquor; In mixed liquor, add 7g ptfe emulsion (polytetrafluoroethylene (PTFE) concentration is 50%), by supersonic oscillations (frequency 53KHz, 20 minutes), ptfe emulsion is mixed with mixed liquor, then leave standstill to bubble collapse, obtain dispersion and to mix liquid;
Liquid is collected in b, preparation: be that the dimethicone of 500 centipoises mixes with 40g thickener (thunder nation chemical industry RB-1200 dimethicone 1,000,000 cs) by 40g viscosity, stir and leave standstill to bubble collapse, obtaining collection liquid, viscosity 100,000 centipoise of collection liquid.
C, preparation continuous phase solution: be that the dimethicone of 500 centipoises is as continuous phase solution using viscosity;
D, 1ml decentralized photo syringe pump decentralized photo solution and continuous phase solution being respectively charged into microfluidic control device and 20ml continuous phase syringe pump, liquid will be collected and load returnable, the flow controlling decentralized photo solution and continuous phase solution is respectively 1ul/min and 100ul/min, and capillary size is internal diameter 252um, external diameter 358um; Decentralized photo flexible pipe 5 and continuous phase flexible pipe 6 are of a size of external diameter 1590um, internal diameter 762um; Outer catheter for deriving drop is of a size of internal diameter 1.6mm, external diameter 3.2mm;
E, starting drive, at the outflow port place of decentralized photo solution, decentralized photo solution is constantly sheared by continuous phase solution, forms the dispersed dispersed phase drop having carbon black;
F, collect dispersed phase drop in returnable collection liquid, and the moisture evaporated by high temperature drying (90 DEG C, 24 hours) in described dispersed phase drop, while making carbon black gather the side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, by the pending Janus microballoon of step f gained from collection liquid take out, washing by soaking is carried out with benzinum in vent cabinet, remove the silicone oil of described pending Janus microsphere surface, and then the benzinum of pending Janus microsphere surface is washed away with ethanol, dry under room temperature, obtain and treat calcining Janus microballoon; The number of times cleaning silicone oil with benzinum is 4 times, to ensure to remove silicone oil completely; It is 2 times with the number of times of ethanol purge benzinum, to ensure to remove benzinum completely.
H, will treat that calcining Janus microballoon carries out high-temperature calcination (300 DEG C, 2 hours), obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and the different in nature feature of optics of size uniformity.
Fig. 7 is the optical microscope picture of thus obtained microsphere, and can find out that microballoon is made up of two hemisphere, the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black is white.Microspherulite diameter is homogeneous, has monodispersity, and particle diameter is 470um.
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature by the mode identical with embodiment 2, difference is: content of carbon black is reduced to 0.03g by 0.1g, and microballoon does not become carbon black part containing carbon black from half containing carbon black half and is less than not containing carbon black part.Can see, reduce the content of carbon black, the microballoon carbon black fraction of gained reduces.The regulation and control of particle diameter pattern can be realized by the content adjusting carbon black.
Embodiment 5
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature as follows:
A, preparation decentralized photo solution: 0.15g carbon black is added in 7g distilled water, within 4 hours, make carbon black dispersion even by planetary ball mill ball milling (revolution speed is 200rpm), obtain mixed liquor; 7g ptfe emulsion (polytetrafluoroethylene (PTFE) concentration is 50%) is added in described mixed liquor, by supersonic oscillations (frequency 53KHz, 20 minutes) ptfe emulsion is mixed with described mixed liquor, then leave standstill to bubble collapse, obtain dispersion and to mix liquid;
Liquid is collected in b, preparation: be that the dimethicone of 500 centipoises mixes with 40g thickener (thunder nation chemical industry RB-1200 dimethicone 1,000,000 cs) by 40g viscosity, stir and leave standstill to bubble collapse, obtaining collection liquid, viscosity 100,000 centipoise of collection liquid.
C, preparation continuous phase solution: be that the dimethicone of 500 centipoises is as continuous phase solution using viscosity;
D, 1ml decentralized photo syringe pump decentralized photo solution and continuous phase solution being respectively charged into microfluidic control device and 20ml continuous phase syringe pump, liquid will be collected and load returnable, the flow controlling decentralized photo solution and continuous phase solution is respectively 1ul/min and 100ul/min, and capillary size is internal diameter 252um, external diameter 358um; Decentralized photo flexible pipe 5 and continuous phase flexible pipe 6 are of a size of external diameter 1590um, internal diameter 762um; Outer catheter for deriving drop is of a size of internal diameter 1.6mm, external diameter 3.2mm;
E, starting drive, at the outflow port place of decentralized photo solution, decentralized photo solution is constantly sheared by continuous phase solution, forms the dispersed dispersed phase drop having carbon black;
F, collect dispersed phase drop in returnable collection liquid, and the moisture evaporated by high temperature drying (90 DEG C, 24 hours) in described dispersed phase drop, while making carbon black gather the side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, by the pending Janus microballoon of step f gained from collection liquid take out, washing by soaking is carried out with benzinum in vent cabinet, remove the silicone oil of described pending Janus microsphere surface, and then the benzinum of pending Janus microsphere surface is washed away with ethanol, dry under room temperature, obtain and treat calcining Janus microballoon; The number of times cleaning silicone oil with benzinum is 4 times, to ensure to remove silicone oil completely; It is 2 times with the number of times of ethanol purge benzinum, to ensure to remove benzinum completely.
H, will treat that calcining Janus microballoon carries out high-temperature calcination (300 DEG C, 2 hours), obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and the different in nature feature of optics of size uniformity.
Fig. 8 is the optical microscope picture of thus obtained microsphere, and can find out that microballoon is made up of two hemisphere, the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere not containing carbon black is white.Microspherulite diameter is homogeneous, has monodispersity, and particle diameter is 470um.
The present embodiment prepares the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature by the mode identical with embodiment 2, difference is: content of carbon black is increased to 0.15g by 0.1g, and microballoon does not become carbon black part more than not containing carbon black part containing carbon black from half containing carbon black half.Can see, increase the mass concentration of carbon black, the microballoon carbon black fraction of gained increases.Comparative example 2,4,5 known, the regulation and control of particle diameter pattern can be realized by the mass concentration of carbon black in adjustment decentralized photo solution.
Claims (6)
1. there is carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of electric charge and optics opposite sex feature, it is characterized in that: described microballoon is made up of two polytetrafluoroethylene (PTFE) hemisphere, and wherein in a polytetrafluoroethylene (PTFE) hemisphere containing carbon black;
Described carbon black/polytetrafluoroethylene (PTFE) Janus the microballoon with electric charge and optics opposite sex feature carries out as follows:
A, preparation decentralized photo solution: carbon black is added in distilled water, make carbon black dispersion even by ball milling, obtain mixed liquor; In described mixed liquor, add ptfe emulsion, by vibration, ptfe emulsion is mixed with described mixed liquor, then leave standstill to bubble collapse, obtain dispersion and to mix liquid;
In described carbon black, distilled water and ptfe emulsion, the mass ratio of polytetrafluoroethylene (PTFE) is: 0.03 ~ 0.2:7:3.5;
Liquid is collected in b, preparation: 1:0.1 ~ 5 in mass ratio, mix dimethicone with silicone oil thickener, stir and leave standstill to bubble collapse, obtaining collection liquid;
C, preparation continuous phase solution: using dimethicone as continuous phase solution;
D, decentralized photo solution and continuous phase solution are passed into microfluidic control device, the flow controlling decentralized photo solution and continuous phase solution is respectively 1 ~ 10ul/min and 50 ~ 200ul/min;
E, outflow port place at decentralized photo solution, decentralized photo solution is constantly sheared by continuous phase solution, forms the dispersed dispersed phase drop having carbon black;
F, to be collected by described dispersed phase drop in collection liquid that step b prepares, and evaporate the moisture in described dispersed phase drop by high temperature drying, while making carbon black gather the side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, by the pending Janus microballoon of step f gained from collection liquid take out, carry out washing by soaking with benzinum, remove the silicone oil of described pending Janus microsphere surface, and then wash away the benzinum of pending Janus microsphere surface with ethanol, dry under room temperature, obtain and treat calcining Janus microballoon;
H, treat that calcining Janus microballoon carries out high-temperature calcination by described, obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and the different in nature feature of optics of size uniformity.
2. carbon black according to claim 1/polytetrafluoroethylene (PTFE) Janus microballoon, it is characterized in that: by regulating and controlling the flow of decentralized photo solution and continuous phase solution, regulate and control the particle diameter of described dispersed phase drop, thus the particle diameter of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon, obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of size tunable.
3. carbon black according to claim 1/polytetrafluoroethylene (PTFE) Janus microballoon, it is characterized in that: by the mass concentration of carbon black in regulation and control decentralized photo solution, regulate and control the pattern of described dispersed phase drop, thus the pattern of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon, obtain the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of morphology controllable.
4. carbon black according to claim 1/polytetrafluoroethylene (PTFE) Janus microballoon, is characterized in that: the viscosity of described collection liquid is not less than 100,000 centipoises.
5. carbon black according to claim 1/polytetrafluoroethylene (PTFE) Janus microballoon, is characterized in that: in step f, the condition of high temperature drying is: temperature 90 DEG C, 24 ~ 36 hours time.
6. carbon black according to claim 1/polytetrafluoroethylene (PTFE) Janus microballoon, is characterized in that: the condition of the high-temperature calcination in step h is 200 ~ 350 DEG C, 2 ~ 4 hours.
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| CN107572475A (en) * | 2017-07-28 | 2018-01-12 | 西安建筑科技大学 | A kind of preparation method of hollow Janus particles |
| CN114395276A (en) * | 2021-12-30 | 2022-04-26 | 宁波德泰化学有限公司 | Janus structure carbon black and preparation method thereof |
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| CN102653580A (en) * | 2011-03-01 | 2012-09-05 | 河北工业大学 | Preparation method of Janus-structure composite emulsion particle |
| CN103157525A (en) * | 2013-03-26 | 2013-06-19 | 吉林大学 | Preparation method of micro-fluid one-way valve device based on silicon nano-pillar array |
| CN103276439A (en) * | 2013-06-08 | 2013-09-04 | 南京工业大学 | Preparation method of molecular colloidal photonic crystal beads |
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| CN102653580A (en) * | 2011-03-01 | 2012-09-05 | 河北工业大学 | Preparation method of Janus-structure composite emulsion particle |
| CN103157525A (en) * | 2013-03-26 | 2013-06-19 | 吉林大学 | Preparation method of micro-fluid one-way valve device based on silicon nano-pillar array |
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