CN109337099A - It is a kind of based on photoresponse structure can heart inverse reinvent water directional transmissions material and the preparation method and application thereof - Google Patents
It is a kind of based on photoresponse structure can heart inverse reinvent water directional transmissions material and the preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses it is a kind of based on photoresponse structure can heart inverse reinvent water directional transmissions material and the preparation method and application thereof.The water directional transmissions material is the tubular structure with photothermal conversion ability, and the inner wall of the tubular structure modifies thermosensitive hydrogel；The tubular structure is made of support frame and the optical-thermal conversion material being doped in the support frame；The thermosensitive hydrogel is modified by way of free radical polymerization on the inner wall of the tubular structure.Water directional transmissions material provided by the invention, simple, easy to operate with preparing, the prices of raw materials are cheap, are suitable for large-scale production；This generally existing using sunlight, the green energy is a kind of transmission mode of low-carbon green as drive force source；Modulation can be carried out to the speed of water transmission by way of changing intensity of illumination；The direction that can be transmitted by changing direction of illumination with remote control and regulation water；By open and close light source, realization starts and stops water transmission.
Description
Technical field
The present invention relates to it is a kind of based on photoresponse structure can heart inverse reinvent water directional transmissions material and preparation method thereof with answer
With belonging to field of functional materials.
Background technique
Water is controllable, directional transmissions for fields such as water collections, biological detection, sea water desalination and water-oil separatings with very heavy
The theory and realistic meaning wanted, existing water transmission technology are mainly based upon preset surface anisotropy structure and wellability,
Water transmission device preparation process is complicated, and preparation process energy consumption is high, and using inefficiency when its progress water collection, and it is fixed not have water
To the controllability and remote controllability in the direction of transmission, water can not be transmitted and to be started at a distance, be stopped and directionality
Control, this seriously constrains the development of related fields, is unable to satisfy the demand of reality.In all environmental stimuli response sources, light
Can be abundant with it, cheap and green the advantages that, is widely paid close attention to, by certain technological means realize photo-thermal, opto-mechanical and
Therefore the conversion of photoelectricity etc. is studied extensively.
In addition, poly-N-isopropyl acrylamide hydrogel is the extensive thermoresponsive of Recent study, in temperature height
When minimum critical inversion temperature, material itself is exposed due to methyl hydrophobic section, releases and surround around amino and hydroxyl
Hydrone, thus reversible structure occurs and steps on contracting and hydrophobicity variation, and the process has very good invertibity,
When temperature is lower than minimum critical inversion temperature, high molecular material volume and hydrophily are restored.However, poly-N-isopropyl third
Acrylamide hydrogel mechanical stability is poor, difficult forming, simple poly-N-isopropyl acrylamide hydrogel phase transition temperature without
Method is adjusted.
Summary of the invention
The object of the present invention is to provide it is a kind of based on photoresponse structure can heart inverse reinvent water directional transmissions material, which can
It collapses and expands so that the invertibity of inner wall to occur under illumination condition, therefore internal diameter gradually increases, at the same time, wellability can
From hydrophilic to hydrophobic transformation, therefore, water is under the action of Laplace pressure difference and surface wettability anisotropy, more towards internal diameter
Narrow, the more hydrophilic direction in surface is mobile, that is, the direction opposite with direction of illumination is mobile, and the transmission of water, stop and
Direction can be controlled by illumination.
Specifically, it is provided by the present invention based on photoresponse structure can heart inverse reinvent water directional transmissions material, for light
The inner wall of the tubular structure of thermal transition ability, the tubular structure modifies thermosensitive hydrogel.
The internal diameter of the tubular structure after modifying the thermosensitive hydrogel is millimeter rank, and the length is decimetres and rice
It is more than rank；
In a tubular form, internal diameter is millimeter rank to the microstructure of water directional transmissions material i.e. of the present invention, the length is decimetre and
Meter level not more than.
In the water directional transmissions material, the tubular structure is by support frame and the light being doped in the support frame
Hot-cast socket material is made；
The doping of the optical-thermal conversion material can be the 0.01~1.0% of the support frame quality, such as 0.025%.
In the water directional transmissions material, the support frame can be by poly- dimethoxysiloxane, polyethylene, polychlorostyrene second
Alkene, polypropylene, glass, rubber or resin are made, as external support construction；
The optical-thermal conversion material can be redox graphene, carbon nanotube, polypyrrole, polyaniline, polythiophene or nitrogen
Change carbon；
The redox graphene has excellent chemical stability and higher photothermal conversion efficiency, can be by nature
Light is quickly converted to thermal energy, can be obtained by graphene oxide through reduction, also such as electronation, thermal reduction, photoreduction or irradiation
When using electronation, hydrazine hydrate or hydrogen iodide is can be used as reducing agent in the modes such as original.
In the water directional transmissions material, the thermosensitive hydrogel is modified by way of free radical polymerization in the pipe
On the inner wall of shape structure, fitted closely with inner wall.
In the water directional transmissions material, the thermosensitive hydrogel can be poly-N-isopropyl acrylamide hydrogel or poly-
N-isopropyl acrylamide water-setting gum derivative；
The poly-N-isopropyl acrylamide water-setting gum derivative can be repaired for poly-N-isopropyl acrylamide hydrogel end
Jewelry (such as poly- Amino End Group n-isopropyl acrylamide hydrogel, poly bis alkyl n-isopropyl acrylamide hydrogel), poly- N-
Isopropylacrylamide hydrogel block copolymer (such as poly-N-isopropyl acrylamide acrylic copolymer hydrogel) is based on
The copolymer (such as polymethylacrylic acid n-isopropyl acrylamide copolymer aquagel) of n-isopropyl acrylamide.
Water directional transmissions material provided by the invention has the tubular structure of photothermal conversion ability, and inner wall is modified with thermal sensitivity
Macromolecule hydrogel, inside pipe wall occurs reversible internal diameter and expands under illumination condition, hydrophobicity variation, water droplet can towards internal diameter compared with
Small, more hydrophilic direction displacement, that is, the direction transmission opposite with illumination, as shown in Figure 1；Change in direction of illumination
Afterwards, the direction of water droplet transmission also occurs to change accordingly.
Water directional transmissions material of the present invention, can be prepared as follows: the flexible back bone by establishing tubulose, in skeleton
In be premixed into optical-thermal conversion material, the tubular structure with photothermal conversion ability is obtained, in pipe in the way of light initiation polymerization
Inner wall equably modifies the hydrogel macromolecule of thermal sensitivity, can prepare photoresponse water directional transmissions material.
Specifically, the preparation method of the water directional transmissions material provided by the invention, includes the following steps:
(1) in extracapillary precoating coating, it is then coated with the mixing of the support frame and the optical-thermal conversion material
Liquid is soaked in organic solvent after cured, is stripped to obtain the tubular structure with photothermal conversion ability；
The swelling ratio of the coating and the support frame in the organic solvent is different；
(2) thermosensitive hydrogel is modified in the inner wall of the tubular structure with photothermal conversion ability to get arriving
The water directional transmissions material.
In above-mentioned preparation method, in step (1), the coating is coated to obtain by materials described below:
1) water soluble polymer, such as polyethylene glycol, polyacrylamide or polycarbonate；
2) lower melting-point organic solvent, such as paraffin.
In step (1), the mixed liquor is coated by way of dipping；
The cured temperature is 60~120 DEG C, and the time is 0.5~12 hour；
The organic solvent can be tetrahydrofuran, dimethyl sulfoxide, chloroform or acetone；
Since the swelling ratio of the support frame and the coating in the organic solvent is different, so be prepared
Tubular structure can be automatically stripped from the capillary.
When the support frame uses poly- dimethoxysiloxane, commercial Sylagrd 184 silicon rubber A and B can be used
Component is mixing cured to be obtained；
When the optical-thermal conversion material use redox graphene when, removing after the completion of further include by graphene oxide into
The step of row reduction, tubular structure is placed in closed container as will be described, realizes chemistry also by the way that hydrazine hydrate is added in a reservoir
Original, reducing agent include but is not limited to use hydrazine hydrate, it is possible to use hydrogen iodide etc. is used as reducing agent, and reduction mode includes but unlimited
In using electronation, can also heat-treat, photoreduction and irradiation restore.
In above-mentioned preparation method, in step (2), the thermosensitive hydrogel is modified by way of free radical polymerization；
It is preferred that modifying the thermosensitive hydrogel by way of ultraviolet light response free radical polymerization；
The photoinitiator that the free radical polymerization uses can for benzophenone, light initiator -184 (Irgacure 184),
1- hydroxyl cyclohexyl benzophenone or 2- isopropyl thioxanthone.
Specific steps can are as follows: is soaked in the tubular structure in the solution of the photoinitiator, using described light-initiated
The free radical that agent illumination generates causes the polymerization for preparing the monomer of the thermosensitive hydrogel；
When such as using n-isopropyl acrylamide monomer, polyethyleneimine can be added, poly-N-isopropyl third can be adjusted
The minimum phase transition temperature of acrylamide, and increase its deformation quantity.
Water directional transmissions material provided by the invention, tubular structure (such as poly- dimethoxy silicon with photothermal conversion ability
Oxygen alkane/redox graphene tubular structure), inner wall is modified with macromolecule hydrogel (such as poly-N-isopropyl propylene of thermal sensitivity
Amide), inside pipe wall occurs reversible internal diameter and expands under illumination condition, and hydrophobicity variation, water droplet can be smaller towards internal diameter, more hydrophilic
Direction displacement, that is, opposite with illumination direction transmission.After direction of illumination change, the direction of water droplet transmission is also sent out
Raw corresponding variation.Water directional transmissions material provided by the invention, simple, easy to operate with preparing, the prices of raw materials are cheap, fit
For being mass produced；This generally existing using sunlight, the green energy is a kind of low-carbon green as drive force source
Transmission mode；Modulation can be carried out to the speed of water transmission by way of changing intensity of illumination；By changing direction of illumination
The direction that can be transmitted with remote control and regulation water；By open and close light source, realization starts and stops water transmission.
Detailed description of the invention
Fig. 1 be based on photoresponse structure can heart inverse reinvent water directional transmissions schematic diagram.
Fig. 2 be it is prepared by the present invention based on photoresponse structure can heart inverse reinvent water directional transmissions material micro-structure diagram.
Fig. 3 be it is prepared by the present invention based on photoresponse structure can heart inverse reinvent water directional transmissions material section optics it is (left
Figure) and electron scanning micrograph (right figure).
Fig. 4 is the situation of change of the internal diameter of water directional transmissions material prepared by the present invention under different illumination intensity.
Fig. 5 be it is prepared by the present invention based on photoresponse structure can heart inverse reinvent water directional transmissions material transmittance curve.
The outer wall of water directional transmissions material prepared by the present invention and poly- dimethoxysiloxane under Fig. 6 different illumination intensity
The ramp case of pipe and temperature decline situation after turning off the light.
Fig. 7 is the situation of change of the inner wall affinity of water directional transmissions material prepared by the present invention under different illumination intensity.
Fig. 8 is the digital photograph of photoresponse water directional transmissions (water transmission direction accordingly changes after changing direction of illumination).
Fig. 9 is the speed that different illumination intensity is lauched the directional transmissions in water directional transmissions material prepared by the present invention.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1, based on photoresponse structure can heart inverse reinvent water directional transmissions material preparation
The present embodiment is using redox graphene as optical-thermal conversion material.
Graphene oxide is prepared according to the Hummers method of improvement: accurately weighing 2.5g phosphorus pentoxide and 2.5g over cure
Sour potassium is added into 250mL conical flask, and the concentrated sulfuric acid that 20mL is added under conditions of being stirred continuously will mix with this condition
Object is heated to 80 DEG C, and 3g graphite powder is added thereto, and the partial size of graphite powder is 320 mesh, is added in the case where being stirred continuously
After being heated to 80 DEG C, 3g graphite powder is slowly added into solution for the 20mL concentrated sulfuric acid, and continuous heating stirs 4.5 hours at 80 DEG C,
After the completion of heating, cooling is stood at room temperature.700mL deionized water is added under conditions of continuous heating stirring, and keeps solution
Temperature is no more than 80 DEG C in the whole process, and the excessive concentrated sulfuric acid, 60 DEG C of drying are removed by suction filtration under vacuum.The pre- oxygen dried
The graphite powder of change is added in the concentrated sulfuric acid of 120mL, 15g potassium permanganate is added thereto, and monitor reacting liquid temperature in real time not
More than 80 DEG C, persistently stir 2 hours.It is finally slow added into 20mL hydrogen peroxide (30wt%), the color of mixed liquor is by depth at this time
Brown gradually becomes golden yellow, and resulting mixture is filtered and takes out moisture, then the hydrochloric acid for being 15wt% with 400mL mass concentration
Eccentric cleaning, then with quality 1L dilute hydrochloric acid solution (concentrated hydrochloric acid: water (v/v)=1:9) eccentric cleaning, supernatant is removed, retain bottom
Portion's solid cleans obtained solid with a large amount of deionized waters later, until the pH value of cleaning solution reaches 7.Above-mentioned gained is consolidated
Body is dispersed back into deionized water, and ultrasound removing 1 hour, obtains finely dispersed graphene oxide water dispersion under 120W power
Liquid, the dispersion liquid is in 3000rpmmin-1Revolving speed under be centrifuged 30 minutes, the unstripped graphite powder of lower layer is removed, supernatant is retained
Liquid, and be transferred in bag filter, it dialyses at least two weeks, until the pH value of external dialyzate reaches 7, is seen with atomic force microscope
It examines, gained graphene oxide is 1~2 layer.Obtained graphene oxide dispersion is transferred in clean culture dish, uses liquid nitrogen
Freezing, is placed in freeze-dryer and is lyophilized, gained foam re-ultrasonic dispersion is configured to 5mg mL into tetrahydrofuran solution-1
Solution.
(1) preparation of the tubular structure with photothermal conversion ability
Support frame uses poly- dimethoxysiloxane.
Commercial 184 silicon rubber A of Sylagrd and B component are weighed according to the mass ratio of 10:1 and mixed, 5mL is added thereto
Graphene oxide tetrahydrofuran dispersion liquid (5mg mL-1).After being sufficiently stirred, in vacuum drier, vacuumize, deaeration.
At the same time, 8g polyethylene glycol solid is distributed in 72g deionized water, closed, 100 DEG C of heating water baths 12 are small
When, it is configured to the aqueous solution that mass concentration is 10%, is uniformly applied on capillary glass tube with the mode of dipping, 60 DEG C of bakings
It is dry.
By the resulting capillary glass tube for being coated with polyethylene glycol by the way of dipping, above-mentioned poly- dimethoxy is uniformly coated
The mixed liquor of siloxanes and graphene oxide, 60 DEG C solidify 2 hours.
After solidification, the obtained capillary glass tube coated with poly- dimethoxysiloxane/graphene oxide is immersed in
About 3 minutes in tetrahydrofuran solvent, since the swelling ratio of silicon rubber and polyethylene glycol in tetrahydrofuran dispersion liquid is different, poly- two
Methoxy radical siloxane/graphene oxide automatically strips.
Poly- dimethoxysiloxane/graphene oxide tubular structure that removing is obtained, is placed in closed container, Xiang Qi
The middle 5 drop hydrazine hydrates that are added are restored, and are reacted 2 hours at 90 DEG C, are obtained the poly- dimethoxy silicon oxygen with photothermal conversion ability
Alkane/redox graphene tubular structure, wherein the amount of redox graphene is poly- dimethoxysiloxane quality
0.025%.
(2) poly- dimethoxysiloxane/redox graphene tubular structure inner wall modifies thermosensitive hydrogel
Using n-isopropyl acrylamide hydrogel as thermosensitive hydrogel.
By 2.264gN- N-isopropylacrylamide monomer, 250mg crosslinking agent (N ' N- methylene-bisacrylamide) and 500mg
Polyethyleneimine (average molecular mass 1750gmol-1) be dissolved in deionized water, nitrogen deaeration 30 minutes.
Benzophenone is dissolved in acetone at the same time, 20wt% solution is made, poly- dimethoxy prepared by step (1)
Siloxanes/redox graphene pipe is immersed in the solution 30 minutes, is respectively washed three times after taking-up with ethyl alcohol and water, removal
Unreacted benzophenone.
By above-mentioned n-isopropyl acrylamide monomer, polyethyleneimine (average molecular mass 1750gmol-1) and N ' N-
Methylene-bisacrylamide aqueous solution pours into the tubular structure after impregnating, and irradiates 30 minutes under ultraviolet light, and uv power is
75mWcm-2.Ultraviolet excitation benzophenone, generates free radicals, and causes the polymerization of n-isopropyl acrylamide monomer.It is therein poly-
Aziridine can adjust the minimum phase transition temperature of poly-N-isopropyl acrylamide, and increase its deformation quantity, and polymerization is completed
Unreacted n-isopropyl acrylamide monomer is cleaned with deionized water afterwards, realizes tubular structure inner wall thermoresponsive water-setting
The modification of glue.
The microstructure of water directional transmissions material manufactured in the present embodiment is as shown in Fig. 2, have the poly- of photothermal conversion ability
Dimethoxysiloxane and redox graphene tubular structure, the tubular structure inner wall are modified by way of light initiation polymerization
It is upper that there is n-isopropyl acrylamide hydrogel.
The tubular structure internal diameter of water directional transmissions material prepared by the present invention is other in the micron-scale, and length is other in decimetre and meter level
More than.
As shown in figure 3, photoresponse water directional transmissions material manufactured in the present embodiment is lower than under critical inversion temperature
Water contact angle is 30~40 °, and higher than between 80~110 ° of water contact angle under critical inversion temperature, internal diameter is arrived at 250 microns
Between 2000 microns.
Photoresponse water directional transmissions material manufactured in the present embodiment carries out morphology characterization, as shown in figure 3, from optical photograph
It can be seen that, poly-N-isopropyl acrylamide hydrogel is coated uniformly on poly- dimethoxysiloxane/reduction-oxidation in (left figure)
On graphene tubulose inner structural wall, thickness is about 50 microns.From scanning electron microscope diagram (right figure) as can be seen that the water of preparation
Gel shows porous structure, and after irradiating 30s, since guttation occurs for hydrogel, material recurring structure collapses, more
Pore structure is changed into more closely knit structure, and thus the diameter of water transmitting device is extended to about 490 microns (Fig. 4) by 425 microns.
To poly- dimethoxysiloxane/reduction manufactured in the present embodiment coated with poly-N-isopropyl acrylamide hydrogel
Graphene oxide tubular structure absorbance is tested, it can be seen that, has about 80%, visible light in ultra-violet (UV) band by Fig. 5
60% and absorption of the near infrared region close to 100%, illustrate that tubular structure has excellent sun light absorpting ability.
It is coated with poly- dimethoxysiloxane/redox graphene tubulose of poly-N-isopropyl acrylamide hydrogel
Structure is respectively in 50mWcm-2、100mWcm-2And 150mWcm-2Sunlight under irradiate, with infrared thermoviewer it can be seen that, pipe
Temperature be increased to 48 DEG C, 55 DEG C and 62 DEG C (Fig. 6,3 curves above) respectively by room temperature, show poly- dimethoxy silicon oxygen
Alkane/redox graphene tubular structure has very good photothermal conversion ability.To the poly- N- isopropyl of inner wall of the pipe modification
Base acrylamide gel wellability carries out characterization discovery, equally under the conditions of sunlight irradiation, the wellability of inner wall of the pipe by
Initial about 34 ° are increased to about 108 ° (Fig. 7), and hydrophobization occurs to irradiate side in light.
The test of photoresponse water directional transmissions:
By photoresponse water directional transmissions material manufactured in the present embodiment, fix in the plane.With microsyringe, Xiang Guanzhong
0.3 microlitre of deionized water is injected, is placed in 25 DEG C of environment temperature of environment, the sun optical analog for being 2 centimetres with spot size
Device irradiates water droplet side, with the migration situation of high-speed camera record water droplet.Comparative test be poly- dimethoxysiloxane pipe and
Poly- dimethoxysiloxane/redox graphene pipe, as shown in fig. 6, the pipe containing redox graphene has well
Photothermal conversion effect, the poly- dimethoxysiloxane pipe that the curve of bottom represents in opposite figure do not show any light
Thermal effect (100mWcm-2Sunlight irradiation under).As a result as shown in figure 8, using water directional transmissions material manufactured in the present embodiment
When, under illumination condition, the negative side of water droplet towards illumination marches forward, and when changing direction of illumination, the direction of motion of water droplet occurs to turn
Become, the maximum speed of water droplet is 1.5mm s-1.As shown in Figure 9.The speed of water droplet can be adjusted by incident intensity, luminous intensity
Bigger, the speed of water droplet directional transmissions is bigger, at any time the propulsion of time, and speed reaches maximum value, and is gradually distance from light source, this
When water drip rate fall to 0 rapidly.
Claims (10)
1. it is a kind of based on photoresponse structure can heart inverse reinvent water directional transmissions material, it is characterised in that: the water directional transmissions material
Material is the tubular structure with photothermal conversion ability, and the inner wall of the tubular structure modifies thermosensitive hydrogel.
2. water directional transmissions material according to claim 1, it is characterised in that: the tubular structure is by support frame and mixes
The miscellaneous optical-thermal conversion material in the support frame is made；
The doping of the optical-thermal conversion material is the 0.01~1.0% of the support frame quality.
3. water directional transmissions material according to claim 2, it is characterised in that: the support frame is by poly- dimethoxy silicon
Oxygen alkane, polyethylene, polyvinyl chloride, polypropylene, glass, rubber or resin are made；
The optical-thermal conversion material is redox graphene, carbon nanotube, polypyrrole, polyaniline, polythiophene or carbonitride.
4. water directional transmissions material according to any one of claim 1-3, it is characterised in that: the thermosensitive hydrogel
It is modified by way of free radical polymerization on the inner wall of the tubular structure.
5. water directional transmissions material described in any one of -4 according to claim 1, it is characterised in that: the thermosensitive hydrogel
For poly-N-isopropyl acrylamide hydrogel or poly-N-isopropyl acrylamide water-setting gum derivative.
6. the preparation method of water directional transmissions material, includes the following steps: described in any one of claim 1-5
(1) in extracapillary precoating coating, it is then coated with the mixed liquor of the support frame and the optical-thermal conversion material, is passed through
It is soaked in organic solvent after solidification, is stripped to obtain the tubular structure with photothermal conversion ability；
The swelling ratio of the coating and the support frame in the organic solvent is different；
(2) thermosensitive hydrogel is modified to get described in the inner wall of the tubular structure with photothermal conversion ability
Water directional transmissions material.
7. preparation method according to claim 6, it is characterised in that: in step (1), coated by way of dipping described
Mixed liquor；
The cured temperature is 60~120 DEG C, and the time is 0.5~12 hour；
The organic solvent is tetrahydrofuran, dimethyl sulfoxide, chloroform or acetone.
8. preparation method according to claim 6 or 7, it is characterised in that: in step (2), pass through the side of free radical polymerization
Formula modifies the thermosensitive hydrogel.
9. preparation method according to claim 8, it is characterised in that: repaired by way of ultraviolet light response free radical polymerization
Adorn the thermosensitive hydrogel；
The photoinitiator that the free radical polymerization uses is different for benzophenone, light initiator -184,1- hydroxyl cyclohexyl benzophenone or 2-
Propyl thioxanthone.
10. application of the water directional transmissions material described in any one of claim 1-5 in following:
The directional transmissions of water are driven under light illumination.
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| CN105816881A (en) * | 2015-12-29 | 2016-08-03 | 温州生物材料与工程研究所 | Composite system based on near-infrared photothermal agent and temperature-sensitive polymer, drug carrier and preparation method |
| CN107033279A (en) * | 2017-05-22 | 2017-08-11 | 深圳先进技术研究院 | A kind of deformable stimuli responsive material and preparation method thereof and stimuli responsive flexible microelectrode arrays |
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