CN107376006A - A kind of preparation method of porous artificial skin receptor - Google Patents
A kind of preparation method of porous artificial skin receptor Download PDFInfo
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- CN107376006A CN107376006A CN201710626794.6A CN201710626794A CN107376006A CN 107376006 A CN107376006 A CN 107376006A CN 201710626794 A CN201710626794 A CN 201710626794A CN 107376006 A CN107376006 A CN 107376006A
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- polyester
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- artificial skin
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- porous artificial
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/08—Carbon ; Graphite
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/28—Materials for coating prostheses
- A61L27/30—Inorganic materials
- A61L27/306—Other specific inorganic materials not covered by A61L27/303 - A61L27/32
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/56—Porous materials, e.g. foams or sponges
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L27/60—Materials for use in artificial skin
Abstract
The present invention relates to receptor field, discloses a kind of preparation method of porous artificial skin receptor, including：(1) graphene is acidified；(2) wiring solution-forming；(3) polyester is dissolved in the concentrated sulfuric acid；(4) inverse emulsion system is made in n-hexane, deionized water, AEO and PEG 400；(5) polyester liquid is added in emulsion, a layer suspension is removed after standing, neutralized；(6) micron order polyester microsphere is made；(7) polyester microsphere solution is mixed with graphene, film, dried；(8) to the processing of graphene polyester compound film, then soaked in solvent dissolve polyester；(9) composite membrane communications and liaison ammonia gas is reduced；(10) it is silver-plated, obtain porous artificial skin receptor.Porous artificial skin receptor produced by the present invention has porous, good permeability；There is excellent electric conductivity, electrochemistry sensitiveness, toughness, intensity and tensile property simultaneously.
Description
Technical field
The present invention relates to receptor field, more particularly to a kind of preparation method of porous artificial skin receptor.
Technical background
Artificial skin is a kind of dressing for being used to treat skin trauma, mainly uses biomaterial or good biocompatibility
Synthetic material be prepared.Artificial skin medical field to scald, burn and skin injury missing play the role of it is good,
Even can be as the substitute of natural skin under certain situation.The artificial skin succeeded in developing and applied at present primarily serves
The covering effect of certain protection hypodermis, there is provided promote the composite material bracket of surface of a wound epidermal growth, or have
Some can promote the slow releasing pharmaceutical factor of skin growth.This kind of artificial skin has good biocompatibility, physical mechanical
Performance and medical performance, but its production is complicated, cost is high and the sense of touch impression without natural skin and signal transmit work(
Energy.
Artificial skin receptor is that environmental stimuli perceptional function and electric signal are added on the basis of original artificial skin
Transmit the membranaceous composite of function.This kind of receptor has certain perceptional function with the change to external environment and stimulation,
As thermoreceptor can perceive the change of skin temperature, thigmoreceptor can perceive the deformation that external force acts on lower skin.Stone
Black alkene is typically used to synthesize artificial skin, but the artificial skin that at present prepared by graphene because its good electrochemistry sensitiveness
Skin receptor common problem is that physical and mechanical properties and gas permeability are not up to requirement.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of preparation method of porous artificial skin receptor.This
Invention prepares film forming using the graphene of good biocompatibility, is gone by the method for adding polyester microsphere and dissolving after shaping
Except polyester, porous graphene film has just been obtained.Porous graphene film has excellent permeability, and loose structure
It is easy to load other active principles during post-processing.Graphene has excellent electric conductivity and electrochemistry sensitiveness, especially
After silver is plated, in the lower size that can change resistance of external force, within the specific limits with excellent intensity and draftability
Energy.And use the method post-processed again after film forming to avoid the reunion of single-layer graphene, toughness is effectively increased, overcomes biography
System graphene film receptor common problem.
The present invention concrete technical scheme be：A kind of preparation method of porous artificial skin receptor, comprises the following steps：
(1) carry out boiling after taking the ground crushing of graphene, in addition salpeter solution and boil processing 20-60 minutes, centrifuge washing.
(2) take the graphene after part centrifugal to dry and weigh measure concentration, then according to the concentration measured to remaining graphite
Alkene adds deionized water wiring solution-forming.
In step (2), graphene cannot pass through drying process, but obtain the concentration of graphene sample using sampling and measuring
Then certain density solution is configured to again.The reunion of graphene can be so reduced, improves the transparency of finished product.
(3) 2-5g polyester pelletizings are dissolved in the 90-110mL concentrated sulfuric acids, stood in unglazed place, until polyester is completely dissolved.
(4) 150-250mL n-hexanes, 100-200mL deionized waters, 5-10mL poly alkyl alcohols are added in three-necked flask
Oxygen vinethene and 2-4mLPEG-400 are quickly stirred, and inverse emulsion system is made.
(5) polyester liquid prepared is instilled in emulsion under agitation, after the entry to be completely, stops stirring, it is quiet
Postpone and remove a layer suspension, add sodium hydroxide and neutralize.
(6) deionized water centrifuge washing is added in the suspension become reconciled in 3-5 times, until there is no sulfate radical in supernatant
Ion, water is then added to lower sediment and is freeze-dried, micron order polyester microsphere is made.
Need to be freeze-dried after adding a certain amount of water to precipitation, freeze-drying can prevent polyester microsphere from reuniting.
(7) polyester microsphere is configured to 0.1g/L-0.5g/L solution, then mixed graphene and polyester microsphere solution
Close, ultrasonic disperse, form graphene-polyester compound film using spin-coating method, as conductive layer, be dried.
(8) with 20-50mL 0.1-1mol/L HCl solutions is handled to graphene-polyester compound film 10-20 minutes, then
It is 0.8-1.2 that composite membrane is immersed in into volume ratio:Stood in 1 phenol tetrachloroethane solvent, dissolve polyester；
(9) dried film is passed through hydrazine gas under the conditions of 110-130 DEG C, the graphene in film is reduced into reduction graphite
Alkene.
(10) last layer silverskin is plated to reduced graphene film using vapour deposition process, obtains porous artificial skin receptor.
Nano Silver has good electrochemistry sensitiveness, can improve the sensitivity of artificial skin receptor.
The present invention carries out reduction treatment after the film was formed by the way that graphene and polyester are fabricated into artificial skin, obtains
Porous artificial skin film.Compared with prior art, this method environmental pollution is small, and preparation method is simple.Manufactured artificial skin
Receptor electric conductivity, good permeability, there is good outer force-responsive and physical and mechanical properties.
Preferably, in step (1), the solid-to-liquid ratio of graphene and salpeter solution is 0.1g:100mL-0.5g:100mL, nitre
The concentration of acid solution is 0.1-1mol/L.
The electric conductivity of graphene is improved after pernitric acid acidification, while the translucency of graphene film will not be because
This and change.
Preferably, in step (3), the concentration of the concentrated sulfuric acid is 98wt%, and the concentration of ordinary dissolution of polyester is less than 5g/L；It is molten
It is 3-4 days to solve the time.Under the conditions of above-mentioned parameter, it can ensure that polyester can be completely dissolved.The concentrated sulfuric acid is poly- compared at present
Ester solvent has no irritating odor, and solubility property is preferable.
Preferably, in step (4), the n-hexane, deionized water, AEO and PEG-40 volume
Than for 65-85:40-60:1.5-2.5:1.
Preferably, in step (5), polyester liquid is slowly added in emulsion under condition of ice bath, and stir speed (S.S.) control exists
2000-3000r/min, the drop rate of polyester liquid is the 0.25-0.50mL/ seconds.
Polyester liquid needs to be slowly added in emulsion under condition of ice bath, to prevent from causing system because of the addition of the concentrated sulfuric acid
Temperature it is too high.The drop rate of polyester liquid needs strict control, to ensure to produce micron order polyester microsphere.
Preferably, in step (7), the mass ratio of graphene and polyester is 15:1-25:1, the ultrasonic disperse time is 20-
30min, drying temperature are 30-60 DEG C.
Preferably, in step (9), the time that is passed through of hydrazine gas is 8-12h.
The graphene that can make to be combined on film that is passed through of hydrazine gas is reduced into electric conductivity and preferably reduces stone
Black alkene.Meanwhile after artificial skin film restores processing after film forming, the agglomeration of graphene can also be effectively prevented,
Improve the transparency of film.
Preferably, in step (4), mixing speed 2000-3000r/min.
Preferably, in step (8), composite membrane stands 20-28h in phenol tetrachloroethane solvent.
It is compared with the prior art, the beneficial effects of the invention are as follows：
(1) present invention removes polyester again using graphene and polyester microsphere mixing film forming, obtains the method for porous graphene, product
One-tenth porosity is big, and gas permeability is excellent.
(2) present invention restores processing method after using graphene film forming, and product has excellent transparency, well simultaneously
External force response performance and physical and mechanical properties.
(3) present invention is acted on simultaneously using graphene and silver, and chemical property is sensitive.
(4) present invention is less using chemicals, and experimentation is green.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of preparation method of porous artificial skin receptor, using following steps：
(1) 0.5g graphenes are taken after grinding, carrying out boiling in addition 0.1mol/L salpeter solutions boils processing 60 minutes, from
The heart washs.
(2) take the graphene after appropriate centrifugation to dry and weigh measure concentration, and add deionized water to be made into 4mg/mL concentration
Solution.
(3) 2g polyester pelletizings are dissolved in the 50mL 98wt% concentrated sulfuric acids, is placed on unglazed place and stands 2 days, until polyester is complete
Dissolving.
(4) added in three-necked flask 150mL n-hexanes, 100mL deionized waters, 5mL AEOs and
2mLPEG-400 is quickly stirred（2500r/min）, inverse emulsion system is made.
(5) polyester liquid prepared is slowly added in emulsion with 1 drop/sec of speed, after the entry to be completely, stops stirring
Mix, a layer suspension is removed after standing, add 0.1mol/L sodium hydroxides and neutralize.Wherein, stir speed (S.S.) is controlled in 2500r/min,
The drop rate of polyester liquid is the 0.40mL/ seconds.
(6) suspension become reconciled in adds deionized water and carries out centrifuge washing 3-5 times, until not having sulfuric acid in supernatant
Radical ion, then it is freeze-dried, micron order polyester microsphere is made.
(7) take a certain amount of polyester microsphere to be configured to 0.1g/L solution, graphene and polyester are then pressed certain 15:1 matter
Amount is than mixing, ultrasonic disperse, wherein, the ultrasonic disperse time be 25min, and drying temperature is 45 DEG C, then using spin-coating method film forming,
As conductive layer, dry at room temperature.
(8) graphene-polyester compound film is handled 10 minutes with 20mL 0.1mol/LHCl solution, then by composite membrane
It is immersed in phenol tetrachloroethane 1:24h is stood in 1 solvent, dissolves polyester.
(9) film being cleaned and dried is passed through to hydrazine gas 8h under the conditions of 120 DEG C, the graphene in film is reduced into also
Former graphene.
(10) last layer silverskin is plated to reduced graphene film using vapour deposition process, obtains porous artificial skin receptor.
Embodiment 2
A kind of preparation method of porous artificial skin receptor, using following steps：
(1) 0.75g graphenes are taken after grinding, carrying out boiling in addition 0.5mol/L salpeter solutions boils processing 70 minutes,
Centrifuge washing.
(2) take the graphene after appropriate centrifugation to dry and weigh measure concentration, and add deionized water to be made into 3mg/mL concentration
Solution.
(3) 3g polyester pelletizings are dissolved in the 75mL 98wt% concentrated sulfuric acids, is placed on unglazed place and stands 2 days, until polyester is complete
Dissolving.
(4) 200mL n-hexanes, 150mL deionized waters, 8mL AEOs and 3mL are added in three-necked flask
PEG-400 is quickly stirred（2000r/min）, inverse emulsion system is made.
(5) polyester liquid prepared is slowly added in emulsion with 2 drops/sec of speed, after the entry to be completely, stops stirring
Mix, a layer suspension is removed after standing, add 0.2mol/L sodium hydroxides and neutralize.Wherein, stir speed (S.S.) is controlled in 2000r/min,
The drop rate of polyester liquid is the 0.25mL/ seconds.
(6) suspension become reconciled in adds deionized water and carries out centrifuge washing 3-5 times, until not having sulfuric acid in supernatant
Radical ion, then it is freeze-dried, micron order polyester microsphere is made.
(7) take a certain amount of polyester microsphere to be configured to 0.2g/L solution, graphene and polyester are then pressed certain 20:1 matter
Amount is than mixing, ultrasonic disperse, wherein, the ultrasonic disperse time be 20min, and drying temperature is 60 DEG C, then using spin-coating method film forming,
As conductive layer, dry at room temperature.
(8) graphene-polyester compound film is handled 20 minutes with 30mL 0.2mol/LHCl solution, then by composite membrane
It is immersed in phenol tetrachloroethane 1:28h is stood in 1 solvent, dissolves polyester.
(9) film being cleaned and dried is passed through to hydrazine gas 9h under the conditions of 120 DEG C, the graphene in film is reduced into also
Former graphene.
(10) last layer silverskin is plated to reduced graphene film using vapour deposition process, obtains porous artificial skin receptor.
Embodiment 3
A kind of preparation method of flexible and transparent artificial skin receptor, using following steps：
(1) 1.0g graphenes are taken after grinding, carrying out boiling in addition 1.0mol/L salpeter solutions boils processing 70 minutes, from
The heart washs.
(2) take the graphene after appropriate centrifugation to dry and weigh measure concentration, and add deionized water to be made into 2mg/mL concentration
Solution.
(3) 5g polyester pelletizings are dissolved in the 100mL 98wt% concentrated sulfuric acids, is placed on unglazed place and stands 3 days, until polyester is complete
Dissolving.
(4) added in three-necked flask 250mL n-hexanes, 200mL deionized waters, 8mL AEOs and
4mLPEG-400 is quickly stirred（3000r/min）, inverse emulsion system is made.
(5) polyester liquid prepared is slowly added in emulsion with 2 drops/sec of speed, after the entry to be completely, stops stirring
Mix, a layer suspension is removed after standing, add 0.5mol/L sodium hydroxides and neutralize.Wherein, stir speed (S.S.) is controlled in 3000r/min,
The drop rate of polyester liquid is the 0.50mL/ seconds.
(6) suspension become reconciled in adds deionized water and carries out centrifuge washing 3-5 times, until not having sulfuric acid in supernatant
Radical ion, then it is freeze-dried, micron order polyester microsphere is made.
(7) take a certain amount of polyester microsphere to be configured to 0.5g/L solution, graphene and polyester are then pressed certain 25:1 matter
Amount is than mixing, ultrasonic disperse, wherein, the ultrasonic disperse time be 30min, and drying temperature is 30 DEG C, then using spin-coating method film forming,
As conductive layer, dry at room temperature.
(8) graphene-polyester compound film is handled 20 minutes with 40mL 0.5mol/LHCl solution, then by composite membrane
It is immersed in phenol tetrachloroethane 1:20h is stood in 1 solvent, dissolves polyester.
(9) film being cleaned and dried is passed through to hydrazine gas 10h under the conditions of 120 DEG C, the graphene in film is reduced into
Reduced graphene.
(10) last layer silverskin is plated to reduced graphene film using vapour deposition process, obtains porous artificial skin receptor.
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted；In the present invention
Method therefor, it is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and the equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (9)
1. a kind of preparation method of porous artificial skin receptor, it is characterised in that comprise the following steps：
(1) carry out boiling after taking the ground crushing of graphene, in addition salpeter solution and boil processing 20-60 minutes, centrifuge washing；
(2) take the graphene after part centrifugal to dry and weigh measure concentration, then remaining graphene is added according to the concentration measured
Deionized water wiring solution-forming；
(3) 2-5g polyester pelletizings are dissolved in the 90-110mL concentrated sulfuric acids, stood in unglazed place, until polyester is completely dissolved；
(4) 150-250mL n-hexanes, 100-200mL deionized waters, 5-10mL fatty alcohol polyoxy second are added in three-necked flask
Alkene ether and 2-4mLPEG-400 are quickly stirred, and inverse emulsion system is made；
(5) polyester liquid prepared is instilled in emulsion under agitation, after the entry to be completely, stops stirring, after standing
A layer suspension is removed, sodium hydroxide is added and neutralizes；
(6) deionized water centrifuge washing is added in the suspension become reconciled in 3-5 time, up to do not have in supernatant sulfate radical from
Son, water is then added to lower sediment and is freeze-dried, micron order polyester microsphere is made；
(7) polyester microsphere is configured to 0.1g/L-0.5g/L solution, then mixed graphene and polyester microsphere solution, is surpassed
Sound disperses, and forms graphene-polyester compound film using spin-coating method, as conductive layer, is dried；
(8) with 20-50mL 0.1-1mol/L HCl solutions is handled to graphene-polyester compound film 10-20 minutes, then will be multiple
It is 0.8-1.2 to close film and be immersed in volume ratio:Stood in 1 phenol tetrachloroethane solvent, dissolve polyester；
(9) dried film is passed through hydrazine gas under the conditions of 110-130 DEG C, the graphene in film is reduced into reduction graphite
Alkene；
(10) last layer silverskin is plated to reduced graphene film using vapour deposition process, obtains porous artificial skin receptor.
A kind of 2. preparation method of flexible and transparent artificial skin receptor as claimed in claim 1, it is characterised in that step
(1) in, the solid-to-liquid ratio of graphene and salpeter solution is 0.1g:100mL-0.5g:100mL, the concentration of salpeter solution is 0.1-
1mol/L。
A kind of 3. preparation method of porous artificial skin receptor as claimed in claim 1, it is characterised in that in step (3),
The concentration of the concentrated sulfuric acid is 98wt%, and the concentration of ordinary dissolution of polyester is less than 5g/L；Dissolution time is 3-4 days.
A kind of 4. preparation method of porous artificial skin receptor as claimed in claim 1, it is characterised in that in step (4),
The n-hexane, deionized water, AEO and PEG-40 volume ratio are 65-85:40-60:1.5-2.5:1.
A kind of 5. preparation method of porous artificial skin receptor as claimed in claim 1, it is characterised in that in step (5),
Polyester liquid is slowly added in emulsion under condition of ice bath, and stir speed (S.S.) is controlled in 2000-3000r/min, the drop of polyester liquid
Rate of acceleration is the 0.25-0.50mL/ seconds.
A kind of 6. preparation method of porous artificial skin receptor as claimed in claim 1, it is characterised in that in step (7),
The mass ratio of graphene and polyester is 15:1-25:1, the ultrasonic disperse time is 20-30min, and drying temperature is 30-60 DEG C.
A kind of 7. preparation method of porous artificial skin receptor as claimed in claim 1, it is characterised in that in step (9),
The time that is passed through of hydrazine gas is 8-12h.
A kind of 8. preparation method of porous artificial skin receptor as claimed in claim 1, it is characterised in that in step (4),
Mixing speed is 2000-3000r/min.
A kind of 9. preparation method of porous artificial skin receptor as claimed in claim 1, it is characterised in that in step (8),
Composite membrane stands 20-28h in phenol tetrachloroethane solvent.
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| CN102180463A (en) * | 2011-02-21 | 2011-09-14 | 电子科技大学 | Method for reducing sheet resistance of graphene thin film |
| US20130309776A1 (en) * | 2011-07-22 | 2013-11-21 | The Trustees Of The University Of Pennsylvania | Graphene-Based Nanopore and Nanostructure Devices and Methods for Macromolecular Analysis |
| CN103623817A (en) * | 2013-11-21 | 2014-03-12 | 同济大学 | High durability anode catalyst for vehicle-mounted fuel cell and preparation method of catalyst |
| CN106395802A (en) * | 2016-09-08 | 2017-02-15 | 山东理工大学 | Method for preparing graphene porous membrane |
| CN106458601A (en) * | 2014-06-17 | 2017-02-22 | 埃琳娜·莫洛卡诺瓦 | Graphene and graphene-related materials for manipulation of cell membrane potential |
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2017
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| CN102180463A (en) * | 2011-02-21 | 2011-09-14 | 电子科技大学 | Method for reducing sheet resistance of graphene thin film |
| US20130309776A1 (en) * | 2011-07-22 | 2013-11-21 | The Trustees Of The University Of Pennsylvania | Graphene-Based Nanopore and Nanostructure Devices and Methods for Macromolecular Analysis |
| CN103623817A (en) * | 2013-11-21 | 2014-03-12 | 同济大学 | High durability anode catalyst for vehicle-mounted fuel cell and preparation method of catalyst |
| CN106458601A (en) * | 2014-06-17 | 2017-02-22 | 埃琳娜·莫洛卡诺瓦 | Graphene and graphene-related materials for manipulation of cell membrane potential |
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