CN103920434A - Carbon black/polytetrafluoroethylene Janus microsphere with controllable particle size and morphology and charge and optical anisotropic characteristics and preparation method thereof - Google Patents
Carbon black/polytetrafluoroethylene Janus microsphere with controllable particle size and morphology and charge and optical anisotropic characteristics and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a carbon black/polytetrafluoroethylene Janus microsphere with controllable particle size and morphology and charge and optical anisotropic characteristics and a preparation method thereof. The carbon black/polytetrafluoroethylene Janus microsphere is characterized by being formed by two polytetrafluoroethylene hemispheres by adding carbon black to a dispersed phase solution and controlling the viscosity of a collecting solution, wherein one polytetrafluoroethylene hemisphere contains carbon black and is black, and the other polytetrafluoroethylene hemisphere free of carbon black is white. The prepared carbon black/polytetrafluoroethylene Janus microsphere has an obvious boundary of the polytetrafluoroethylene hemisphere containing carbon black and the other polytetrafluoroethylene hemisphere free of carbon black, and a high degree of sphericity, the polytetrafluoroethylene material can resist a severe environment, and is difficult to react with a chemical reagent, and good in stability, and no water or oil is adhered to the polytetrafluoroethylene material.
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 to be proposed in the Nobel Prize award-giving meeting of 1991 by De Gennes the earliest, derives from the name of a two-sided god in ancient Roman's mythology, and being used for explaining surperficial two hemispheres mask has particle of different nature.Because its two sides has different character, so its application prospect is very extensive, relates to physics, chemistry, biology, 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 for showing the Electronic Paper in field, under extra electric field, by changing direction of an electric field, realize the upset of the particle that both sides color is different, reach the principle of colour developing.
The people such as Daisuke Suzuki, by golden sputtering method, by the local above gold that covers 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 it is more even to be difficult to guarantee fund's distribution.
And micro-fluidic technologies that can control accurate microballoon size is subject to people's attention equally.The double capillary microfluid that adopts microfluidic channel to flow altogether method and Shin-Hyun Kim as Takasi Nisisako flows altogether and cuts into drop with full-bodied two kinds of fluids realizes Janus microballoon.This method need to guarantee that two kinds of liquid that dissolve each other can not spread when parallel flowing, and are therefore difficult to regulate.
Obtaining size can be from tens micron to the regulation and control of hundreds of micron, interface is clear, corrosion-resistant and have electric charge with the microballoon of the optics opposite sex is the direction of scientists effort always.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide a kind ofly by two corrosion resistant polytetrafluoroethylene (PTFE) hemisphere, to be formed and the preparation method of the particle diameter that contains carbon black in a polytetrafluoroethylene (PTFE) hemisphere therein and the controlled carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex characteristic of pattern.
Another object of the present invention is to provide a kind of particle diameter and the controlled carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of pattern.
Technical solution problem of the present invention, adopts following technical scheme:
The preparation method of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature that particle diameter of the present invention and pattern are controlled, its feature is to carry out as follows:
A, preparation decentralized photo solution: carbon black is added in distilled water, by ball milling, make carbon black dispersion even, obtain mixed liquor; In described mixed liquor, add ptfe emulsion, by vibration, ptfe emulsion is mixed with described mixed liquor, then standing to bubble collapse, must disperse the liquid that mixes; After vibration, can make solution surface produce bubble, should be standing re-use to bubble collapse, because bubble can affect the big or small 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, dimethicone is mixed with silicone oil thickener, and stir also standing to bubble collapse, obtain 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 of controlling decentralized photo solution and continuous phase solution is respectively 1～10ul/min and 50～200ul/min;
E, 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 that has carbon black;
F, described dispersed phase drop is collected in the collection liquid that step b prepares, and evaporated the moisture in described dispersed phase drop by high temperature drying, when making carbon black gather a side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon; Because the moisture in drop slowly evaporates, make it finally become microspheres with solid.In this section of process, carbon black can gather a side wherein gradually simultaneously.Because silicon oil viscosity is very large, the sedimentation meeting of drop is very slow, have cured, so sphericity is better before it is deposited to bottom.
G, the pending Janus microballoon of step f gained is taken out from collect liquid, with benzinum, carry out washing by soaking, remove the silicone oil of described pending Janus microsphere surface, and then with ethanol, wash away the benzinum of pending Janus microsphere surface, dry under room temperature, obtain Janus microballoon to be calcined; Preferably, the number of times that cleans silicone oil with benzinum is more than 4 times, to guarantee removing silicone oil completely; The number of times that cleans benzinum with ethanol is more than 2 times, to guarantee removing benzinum completely.
Described in h, general, Janus microballoon to be calcined carries out high-temperature calcination, obtains carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of size homogeneous.
Preparation method of the present invention, its feature is also: by the flow of regulation and control decentralized photo solution and continuous phase solution, regulate and control the particle diameter of described dispersed phase drop, thereby the particle diameter of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon obtains the controlled carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of particle diameter.
By the mass concentration of carbon black in regulation and control decentralized photo solution, regulate and control the pattern of described dispersed phase drop, thereby the pattern of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon obtains the controlled carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of pattern.
Preferably, the viscosity of described collection liquid is not less than 100,000 centipoises.The too low meeting of viscosity of collecting liquid causes droplet settling excessive velocities, makes drop before being cured, just sink to container bottom, makes the bottom of ball occur a flat region.The higher ball sinking speed that can make of viscosity is slack-off, concedes points and just has cured before sinking to bottom, and the sphericity obtaining is better.
Preferably, in step f, the condition of high temperature drying is: 90 ℃ of temperature, 24～36 hours time.
Preferably, the condition of the high-temperature calcination in step h is 200～350 ℃, 2～4 hours.Temperature is higher than 400 ℃, and polytetrafluoroethylene (PTFE) can decompose.
The present invention further provides the carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature obtaining by above-mentioned preparation method, its feature is: described microballoon consists of two polytetrafluoroethylene (PTFE) hemisphere, and in a polytetrafluoroethylene (PTFE) hemisphere, contains carbon black therein.The polytetrafluoroethylene (PTFE) hemisphere that contains carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is not white in color.
Carbon black/polytetrafluoroethylene (PTFE) Janus microspherulite diameter with electric charge and optics opposite sex feature that preparation method of the present invention obtains is 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 present invention is prepared has in carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of electric charge and optics opposite sex feature containing the polytetrafluoroethylene (PTFE) hemisphere of carbon black with the line of demarcation containing the polytetrafluoroethylene (PTFE) hemisphere of carbon black is unobvious, sphericity is better, polytetrafluoroethylmaterial material can be resisted adverse circumstances, and can not glue water and oil, difficult and chemical reagent reacts, and stability is better;
2, the prepared carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of the present invention is because two hemisphere are all polytetrafluoroethylene (PTFE) materials, and interhemispheric adhesion is very tight, is difficult to disconnect;
3, the present invention is by regulating the speed of decentralized photo and continuous phase, can make the mono-dispersion microballoon of different sizes, microballoon size can reach tens to hundreds of micron, widened electric charge-optical anisotropy microballoon as the double-colored ball of twisting in the application in electric ink field;
The method of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon that 4, prepared by the present invention, by the mass concentration of carbon black in regulation and control decentralized photo solution, can obtain the controlled carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of pattern, can for the needed resolution adjustment of Electronic Paper, contain the shared ratio in 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 A part of the present invention;
Fig. 3 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of embodiment 1 preparation;
Fig. 4 is the picture that carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of embodiment 1 preparation overturns under electric field;
Fig. 5 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of embodiment 2 preparations;
Fig. 6 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of embodiment 3 preparations;
Fig. 7 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of embodiment 4 preparations;
Fig. 8 is the optical microscope photograph of carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of embodiment 4 preparations;
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
The paper microfluidic control device that once embodiments of the invention adopt.
As shown in Figure 1 and Figure 2, microfluidic control device comprises the continuous phase syringe 4 that is arranged on continuous phase syringe pump 3, is arranged on decentralized photo syringe 2, T-shaped threeway 7 and returnable 9 on decentralized photo syringe pump 1;
Continuous phase syringe 4 is connected with the first port of T-shaped threeway 7 by continuous phase flexible pipe 6;
The second port of T-shaped threeway 7 is communicated with outer catheter 8;
The 3rd port of T-shaped threeway and the second port are on same straight line; The outflow port that is arranged on the capillary 11 in T-shaped threeway is inserted in outer catheter 8 through the second port, flows into port and is connected with the outflow port of decentralized photo flexible pipe 5 through the 3rd port, and the inflow port of decentralized photo flexible pipe 5 is communicated with decentralized photo syringe 2; Output port at 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 fixing by connecting hose 14 with outer catheter 8.
Output duct and continuous phase conduit are selected polyfluortetraethylene pipe; 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 diameters are 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, pack collection liquid 10 into returnable 9, start microfluidic control device, the fltting speed of controlling continuous phase syringe pump 3 and decentralized photo syringe pump 1, decentralized photo solution, through capillary, is located in the outflow port (being the outflow port of decentralized photo solution) of capillary 11, by continuous phase solution, constantly sheared, form the dispersed dispersed phase drop 12 that has 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 converted into solid-state-microspherical by liquid state gradually.Be accompanied by the concentrated solidification process of drop, be dispersed in a side the final carbon black/polytetrafluoroethylene (PTFE) Janus microballoon not forming containing the polytetrafluoroethylene (PTFE) hemisphere of carbon black forming by the polytetrafluoroethylene (PTFE) hemisphere that contains carbon black of black and white that carbon black in dispersed phase drop gathers drop gradually originally.Its preparation principle is: carbon black fine particle is dispersed in ptfe emulsion, and in microfluidic control device, forms the equally distributed ptfe emulsion drop of carbon black.Along with the moisture evaporation in drop solidification process, ion concentration in emulsion improves constantly, cause the zeta potential of carbon black micelle to reduce gradually, finally make carbon black fine particle assemble, and now polytetrafluoroethylene (PTFE) still can stable dispersion in system, until finally form a side containing carbon black, opposite side does not contain the polytetrafluoroethylene (PTFE) microballoon with Janus structure of carbon black.
Decentralized photo solution flows into the capillary in threeway by conduit under the promotion of syringe pump, is subject to forming big or small identical drop one by one from the shearing force of continuous phase, along with continuous phase flow into the container for collecting through outer catheter at port capillaceous.Due to
d
dropand d
capillaryrefer to drop and diameter capillaceous, 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 size capillaceous, and the viscosity of continuous phase and decentralized photo and speed, we can obtain the drop of different sizes.
Below in conjunction with specific embodiment, further set forth related content of the present invention.It is to be noted, these embodiment are only not used in and limit the scope of the invention for the present invention is described, and, after having read content of the present invention, relevant technical staff in the field can make various changes or modification 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 is prepared 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, by planetary ball mill ball milling (revolution speed is 200rpm), within 4 hours, make carbon black dispersion even, 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 standing to bubble collapse, must disperse the liquid that mixes;
Liquid is collected in b, preparation: the dimethicone that by 40g viscosity is 500 centipoises mixes with 40g thickener (the chemical industry RB-1200 of thunder nation dimethicone 1,000,000 cs), stirs also standing to bubble collapse, obtains collection liquid, and the viscosity of collecting liquid is 100,000 centipoises.
C, preparation continuous phase solution: the dimethicone that the viscosity of usining is 500 centipoises is as continuous phase solution;
D, decentralized photo solution and continuous phase solution are respectively charged into 1ml decentralized photo syringe pump and the 20ml continuous phase syringe pump of microfluidic control device, pack collection liquid into returnable, the flow of 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; For deriving the outer catheter of drop, be 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 that has carbon black;
F, dispersed phase drop is collected in the collection liquid in returnable, and by the moisture in high temperature drying (90 ℃, 24 hours) evaporation dispersed phase drop, when making carbon black gather a side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, the pending Janus microballoon of step f gained is taken out from collect liquid, in vent cabinet, with benzinum, carry out washing by soaking, remove the silicone oil of pending Janus microsphere surface, and then with ethanol, wash away the benzinum of pending Janus microsphere surface, dry under room temperature, obtain Janus microballoon to be calcined; The number of times that cleans silicone oil with benzinum is 4 times, to guarantee removing silicone oil completely; The number of times that cleans benzinum with ethanol is 2 times, to guarantee removing benzinum completely.
H, Janus microballoon to be calcined is carried out to high-temperature calcination (300 ℃, 2 hours), obtain carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of size homogeneous.
Fig. 3 is the light microscope picture of thus obtained microsphere, can find out that microballoon is comprised of two hemisphere, and the polytetrafluoroethylene (PTFE) hemisphere that contains carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is not white in color.Microspherulite diameter homogeneous, has monodispersity, and particle diameter is 640um.
Half is black to the optics metamer of thus obtained microsphere now, and half is white.
Electric charge metamer is now as follows: containing the hemisphere of carbon black and not containing the hemisphere of carbon black in external electric field owing to thering is different electrical properties, so can produce electric dipole, microballoon is placed between two electrode plate, add voltage 100V, ball overturns, as shown in Figure 4.
Embodiment 2
The present embodiment is prepared 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, by planetary ball mill ball milling (revolution speed is 200rpm), within 4 hours, make carbon black dispersion even, obtain mixed liquor; In described mixed liquor, add 7g ptfe emulsion (polytetrafluoroethylene (PTFE) concentration is 50%), by supersonic oscillations (frequency 53KHz, 20 minutes) ptfe emulsion is mixed with described mixed liquor, then standing to bubble collapse, must disperse the liquid that mixes;
Liquid is collected in b, preparation: the dimethicone that by 40g viscosity is 500 centipoises mixes with 40g thickener (the chemical industry RB-1200 of thunder nation dimethicone 1,000,000 cs), stirs also standing to bubble collapse, obtains collection liquid, collects viscosity 100,000 centipoises of liquid.
C, preparation continuous phase solution: the dimethicone that the viscosity of usining is 500 centipoises is as continuous phase solution;
D, decentralized photo solution and continuous phase solution are respectively charged into 1ml decentralized photo syringe pump and the 20ml continuous phase syringe pump of microfluidic control device, pack collection liquid into returnable, the flow of 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; For deriving the outer catheter of drop, be 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 that has carbon black;
F, described dispersed phase drop is collected in the collection liquid in returnable, and evaporate the moisture in described dispersed phase drop by high temperature drying (90 ℃, 24 hours), when making carbon black gather a side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, the pending Janus microballoon of step f gained is taken out from collect liquid, in vent cabinet, with benzinum, carry out washing by soaking, remove the silicone oil of described pending Janus microsphere surface, and then with ethanol, wash away the benzinum of pending Janus microsphere surface, dry under room temperature, obtain Janus microballoon to be calcined; The number of times that cleans silicone oil with benzinum is 4 times, to guarantee removing silicone oil completely; The number of times that cleans benzinum with ethanol is 2 times, to guarantee removing benzinum completely.
H, Janus microballoon to be calcined is carried out to high-temperature calcination (300 ℃, 2 hours), obtain carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of size homogeneous.
Fig. 5 is the light microscope picture of thus obtained microsphere, can find out that microballoon is comprised of two hemisphere, and the polytetrafluoroethylene (PTFE) hemisphere that contains carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is not white in color.Microspherulite diameter homogeneous, has monodispersity, and particle diameter is 470um.
The present embodiment is prepared 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 by 50ul/min and is increased to 100ul/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 by adjusting continuous phase flow, can realize the regulation and control of particle diameter.
Embodiment 3
The present embodiment is prepared 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, by planetary ball mill ball milling (revolution speed is 200rpm), within 4 hours, make carbon black dispersion even, 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 standing to bubble collapse, must disperse the liquid that mixes;
Liquid is collected in b, preparation: the dimethicone that by 40g viscosity is 500 centipoises mixes with 40g thickener (the chemical industry RB-1200 of thunder nation dimethicone 1,000,000 cs), stirs also standing to bubble collapse, obtains collection liquid, collects viscosity 100,000 centipoises of liquid.
C, preparation continuous phase solution: the dimethicone that the viscosity of usining is 500 centipoises is as continuous phase solution;
D, decentralized photo solution and continuous phase solution are respectively charged into 1ml decentralized photo syringe pump and the 20ml continuous phase syringe pump of microfluidic control device, pack collection liquid into returnable, the flow of 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; For deriving the outer catheter of drop, be 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 that has carbon black;
F, dispersed phase drop is collected in the collection liquid in returnable, and evaporate the moisture in described dispersed phase drop by high temperature drying (90 ℃, 24 hours), when making carbon black gather a side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, the pending Janus microballoon of step f gained is taken out from collect liquid, in vent cabinet, with benzinum, carry out washing by soaking, remove the silicone oil of described pending Janus microsphere surface, and then with ethanol, wash away the benzinum of pending Janus microsphere surface, dry under room temperature, obtain Janus microballoon to be calcined; The number of times that cleans silicone oil with benzinum is 4 times, to guarantee removing silicone oil completely; The number of times that cleans benzinum with ethanol is 2 times, to guarantee removing benzinum completely.
H, Janus microballoon to be calcined is carried out to high-temperature calcination (300 ℃, 2 hours), obtain carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of size homogeneous.
Fig. 6 is the light microscope picture of thus obtained microsphere, can find out that microballoon is comprised of two hemisphere, and the polytetrafluoroethylene (PTFE) hemisphere that contains carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is not white in color.Microspherulite diameter homogeneous, has monodispersity, and particle diameter is 107um.
The present embodiment is prepared 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 by 100ul/min and is increased to 150ul/min, and the diameter of microballoon is reduced to 107um from 470um.Can see, continue to increase the flow of continuous phase, the microsphere diameter of gained still reduces.Therefore, the known regulation and control that can realize particle diameter by adjusting continuous phase flow of embodiment 1,2,3 contrast.
Embodiment 4
The present embodiment is prepared 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, by planetary ball mill ball milling (revolution speed is 200rpm), within 4 hours, make carbon black dispersion even, 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 standing to bubble collapse, must disperse the liquid that mixes;
Liquid is collected in b, preparation: the dimethicone that by 40g viscosity is 500 centipoises mixes with 40g thickener (the chemical industry RB-1200 of thunder nation dimethicone 1,000,000 cs), stirs also standing to bubble collapse, obtains collection liquid, collects viscosity 100,000 centipoises of liquid.
C, preparation continuous phase solution: the dimethicone that the viscosity of usining is 500 centipoises is as continuous phase solution;
D, decentralized photo solution and continuous phase solution are respectively charged into 1ml decentralized photo syringe pump and the 20ml continuous phase syringe pump of microfluidic control device, pack collection liquid into returnable, the flow of 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; For deriving the outer catheter of drop, be 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 that has carbon black;
F, dispersed phase drop is collected in the collection liquid in returnable, and evaporate the moisture in described dispersed phase drop by high temperature drying (90 ℃, 24 hours), when making carbon black gather a side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, the pending Janus microballoon of step f gained is taken out from collect liquid, in vent cabinet, with benzinum, carry out washing by soaking, remove the silicone oil of described pending Janus microsphere surface, and then with ethanol, wash away the benzinum of pending Janus microsphere surface, dry under room temperature, obtain Janus microballoon to be calcined; The number of times that cleans silicone oil with benzinum is 4 times, to guarantee removing silicone oil completely; The number of times that cleans benzinum with ethanol is 2 times, to guarantee removing benzinum completely.
H, Janus microballoon to be calcined is carried out to high-temperature calcination (300 ℃, 2 hours), obtain carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of size homogeneous.
Fig. 7 is the light microscope picture of thus obtained microsphere, can find out that microballoon is comprised of two hemisphere, and the polytetrafluoroethylene (PTFE) hemisphere that contains carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is not white in color.Microspherulite diameter homogeneous, has monodispersity, and particle diameter is 470um.
The present embodiment is prepared 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 from half, containing carbon black, half does not become carbon black containing carbon black and is partly less than not containing carbon black part microballoon.Can see, reduce the content of carbon black, the microballoon carbon black part ratio of gained reduces.By adjusting the content of carbon black, can realize the regulation and control of particle diameter pattern.
Embodiment 5
The present embodiment is prepared 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, by planetary ball mill ball milling (revolution speed is 200rpm), within 4 hours, make carbon black dispersion even, obtain mixed liquor; In described mixed liquor, add 7g ptfe emulsion (polytetrafluoroethylene (PTFE) concentration is 50%), by supersonic oscillations (frequency 53KHz, 20 minutes) ptfe emulsion is mixed with described mixed liquor, then standing to bubble collapse, must disperse the liquid that mixes;
Liquid is collected in b, preparation: the dimethicone that by 40g viscosity is 500 centipoises mixes with 40g thickener (the chemical industry RB-1200 of thunder nation dimethicone 1,000,000 cs), stirs also standing to bubble collapse, obtains collection liquid, collects viscosity 100,000 centipoises of liquid.
C, preparation continuous phase solution: the dimethicone that the viscosity of usining is 500 centipoises is as continuous phase solution;
D, decentralized photo solution and continuous phase solution are respectively charged into 1ml decentralized photo syringe pump and the 20ml continuous phase syringe pump of microfluidic control device, pack collection liquid into returnable, the flow of 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; For deriving the outer catheter of drop, be 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 that has carbon black;
F, dispersed phase drop is collected in the collection liquid in returnable, and evaporate the moisture in described dispersed phase drop by high temperature drying (90 ℃, 24 hours), when making carbon black gather a side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, the pending Janus microballoon of step f gained is taken out from collect liquid, in vent cabinet, with benzinum, carry out washing by soaking, remove the silicone oil of described pending Janus microsphere surface, and then with ethanol, wash away the benzinum of pending Janus microsphere surface, dry under room temperature, obtain Janus microballoon to be calcined; The number of times that cleans silicone oil with benzinum is 4 times, to guarantee removing silicone oil completely; The number of times that cleans benzinum with ethanol is 2 times, to guarantee removing benzinum completely.
H, Janus microballoon to be calcined is carried out to high-temperature calcination (300 ℃, 2 hours), obtain carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of size homogeneous.
Fig. 8 is the light microscope picture of thus obtained microsphere, can find out that microballoon is comprised of two hemisphere, and the polytetrafluoroethylene (PTFE) hemisphere that contains carbon black is black, and the polytetrafluoroethylene (PTFE) hemisphere containing carbon black is not white in color.Microspherulite diameter homogeneous, has monodispersity, and particle diameter is 470um.
The present embodiment is prepared 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 from half, containing carbon black, half does not become carbon black part more than not containing carbon black part containing carbon black to microballoon.Can see, increase the mass concentration of carbon black, the microballoon carbon black part ratio of gained increases.Comparative example 2,4,5 is known, can realize the regulation and control of particle diameter pattern by adjusting the mass concentration of carbon black in decentralized photo solution.
Claims (8)
1. a preparation method for carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature that particle diameter and pattern are controlled, is characterized in that carrying out as follows:
A, preparation decentralized photo solution: carbon black is added in distilled water, by ball milling, make carbon black dispersion even, obtain mixed liquor; In described mixed liquor, add ptfe emulsion, by vibration, ptfe emulsion is mixed with described mixed liquor, then standing to bubble collapse, must disperse the liquid that mixes;
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, dimethicone is mixed with silicone oil thickener, and stir also standing to bubble collapse, obtain 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 of controlling decentralized photo solution and continuous phase solution is respectively 1～10ul/min and 50～200ul/min;
E, 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 that has carbon black;
F, described dispersed phase drop is collected in the collection liquid that step b prepares, and evaporated the moisture in described dispersed phase drop by high temperature drying, when making carbon black gather a side of dispersed phase drop, dispersed phase drop solidifies, and obtains pending Janus microballoon;
G, the pending Janus microballoon of step f gained is taken out from collect liquid, with benzinum, carry out washing by soaking, remove the silicone oil of described pending Janus microsphere surface, and then with ethanol, wash away the benzinum of pending Janus microsphere surface, dry under room temperature, obtain Janus microballoon to be calcined;
Described in h, general, Janus microballoon to be calcined carries out high-temperature calcination, obtains carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature of size homogeneous.
2. preparation method according to claim 1, it is characterized in that: by the flow of regulation and control decentralized photo solution and continuous phase solution, regulate and control the particle diameter of described dispersed phase drop, thereby the particle diameter of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon, obtains the controlled carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of particle diameter.
3. preparation method according to claim 1, 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, thereby the pattern of regulation and control gained carbon black/polytetrafluoroethylene (PTFE) Janus microballoon, obtains the controlled carbon black/polytetrafluoroethylene (PTFE) Janus microballoon of pattern.
4. preparation method according to claim 1, is characterized in that: the viscosity of described collection liquid is not less than 100,000 centipoises.
5. preparation method according to claim 1, is characterized in that: in step f, the condition of high temperature drying is: 90 ℃ of temperature, 24～36 hours time.
6. preparation method according to claim 1, is characterized in that: the condition of the high-temperature calcination in step h is 200～350 ℃, 2～4 hours.
7. carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature that described in claim 1～6 any one, preparation method obtains.
8. carbon black/polytetrafluoroethylene (PTFE) Janus microballoon with electric charge and optics opposite sex feature according to claim 7, is characterized in that: described microballoon consists of two polytetrafluoroethylene (PTFE) hemisphere, and in a polytetrafluoroethylene (PTFE) hemisphere, contains carbon black therein.
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| 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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