CN106046237B - Carbon fiber paper and the composite conducting gel film and its preparation method of Sodium Polyacrylate and application - Google Patents

Carbon fiber paper and the composite conducting gel film and its preparation method of Sodium Polyacrylate and application Download PDF

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CN106046237B
CN106046237B CN201610369152.8A CN201610369152A CN106046237B CN 106046237 B CN106046237 B CN 106046237B CN 201610369152 A CN201610369152 A CN 201610369152A CN 106046237 B CN106046237 B CN 106046237B
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carbon fiber
fiber paper
gel film
sodium polyacrylate
solution
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CN106046237A (en
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毕见强
赵庆强
王伟礼
孙国勋
王素梅
季红
赵丽霞
高希成
郝旭霞
谢冰莹
邱妍
崔京京
王宁
廖洪芳
段佳琦
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Shandong University
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/04—Acids; Metal salts or ammonium salts thereof
    • C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/02—Details
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61N—ELECTROTHERAPY; MAGNETOTHERAPY; RADIATION THERAPY; ULTRASOUND THERAPY
    • A61N1/00—Electrotherapy; Circuits therefor
    • A61N1/18—Applying electric currents by contact electrodes
    • A61N1/32—Applying electric currents by contact electrodes alternating or intermittent currents
    • A61N1/38—Applying electric currents by contact electrodes alternating or intermittent currents for producing shock effects
    • A61N1/39—Heart defibrillators
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
    • C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
    • C08J3/075—Macromolecular gels
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2333/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Radiology & Medical Imaging (AREA)
  • Biomedical Technology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Cardiology (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paper (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a kind of carbon fiber paper and the composite conducting gel film and its preparation method of Sodium Polyacrylate and application, including Sodium Polyacrylate gel film, the first carbon fiber paper and the second carbon fiber paper, Sodium Polyacrylate gel film forms three layer stacked structures between the first carbon fiber paper and the second carbon fiber paper；Conductive ion solution is adsorbed with Sodium Polyacrylate gel film.It is placed in after the reactant solution mixing of hydrogel between two layers of carbon fiber paper and carries out polymerisation, or after the reactant solution polymerization generation gel film of hydrogel, then between gel film is placed in into two layers of carbon fiber paper, obtains plural gel piece；After plural gel piece is infiltrated into conductive ion solution, composite conducting gel film is obtained.On the one hand carbon fiber paper in composite conducting gel film can improve the mechanical strength of gel film, on the other hand electrically conductive, improve the electric conductivity of gel film jointly with the conductive ion in gel film.

Description

Carbon fiber paper and the composite conducting gel film and its preparation method of Sodium Polyacrylate and application
Technical field
The invention belongs to high polymer material preparation method technical field, more particularly to a kind of carbon fiber paper and Sodium Polyacrylate Composite conducting gel film and its preparation method and application.
Background technology
Since the 1970s finds that polyacetylene is conductive, conducting polymer has turned into researcher and studied Emphasis.So far, most widely used conducting polymer is polyaniline (PANI), polypyrrole (PPy) and polythiophene (PT), this The correlative study of a little conducting polymers has been achieved with larger progress, but there is also it is many shortcomings that, can be right as aniline has severe toxicity Water body pollutes；Pyrroles has serious harm to eyes, sucks or eats and be poisonous；Thiophene foul smelling, these conducting polymers are all It is difficult to apply to have the field of strict demand, such as medical domain to compound property (toxicity, smell etc.).It is therefore desirable to develop The conducting polymer of new " green, nontoxic ".
Polyalcohol hydrogel is typically the polymer water swelling body formed by hydrophilic monomer and crosslinking agent, is a kind of three dimensional network The high molecular polymer of shape structure, belong to typical soft material.Most polymers hydrogel has environment-responsive, i.e., Under environmental stimuli, the response of swelling and deswelling can occur for such as pH, temperature, light and electric field, and this unique property causes Polyalcohol hydrogel is widely used in various functions material, bio-medical material and pharmaceutical carrier etc..
At present, composite conductive polymer hydrogel material enjoys the concern of researcher always recently.In recent years, in life Thing medical domain, using CNT come improve the mechanicalness of hydrogel and electric conductivity be also researcher research focus. But because the Van der Waals force between CNTs is larger, draw ratio is high so that easily produces reunion when generating CNTs.In addition, CNTs Chemical inertness cause its bad dispersibility, it is weak with the effect of the interface cohesion of polymer, significantly limit CNTs application.
The content of the invention
In order to solve problem above present in prior art, it is multiple that the present invention provides a kind of carbon fiber paper/Sodium Polyacrylate Conduction electrocoagulation film is closed, the composite conducting gel film can effectively improve the mechanical performance and electric conductivity of gel film.
It is a further object to provide the system of a kind of carbon fiber paper and the composite conducting gel film of Sodium Polyacrylate Preparation Method.
Third object of the present invention is to provide the preparation system for preparing a kind of composite conducting gel film.
Fourth object of the present invention is to provide answering for the composite conducting gel film of above-mentioned carbon fiber paper and Sodium Polyacrylate With.
In order to solve the above technical problems, the technical scheme is that：
A kind of composite conducting gel film of carbon fiber paper and Sodium Polyacrylate, including Sodium Polyacrylate gel film, the first carbon Fibrous paper and the second carbon fiber paper, Sodium Polyacrylate gel film are formed between the first carbon fiber paper and the second carbon fiber paper Laminated construction；Conductive ion solution is adsorbed with Sodium Polyacrylate gel film.
Three-dimensional network space Sodium Polyacrylate can adsorb certain conductive ion solution, obtain gel film, conductive ion Displacement can occur under energization action, and then form conductive channel, improve the electric conductivity of Sodium Polyacrylate gel film Energy.
First carbon fiber paper and the second carbon fiber paper are separately positioned on to two surfaces up and down of Sodium Polyacrylate gel film, On the one hand support gel rubber piece can be played a part of, improves the mechanical strength of gel film, on the other hand, carbon fiber paper can be led Electricity, the structure of monolithic conductive can be formed together with gel film.
Preferably, the conductive ion solution is sodium chloride solution or Klorvess Liquid, preferably sodium chloride solution.
Sodium chloride solution can parent's profit human body skin, improve the electric conductivity of skin, it is possible to applied in defibrillation procedure The conducting medium of defibrillation electrode and human skin.
It is further preferred that the concentration of the conductive ion is 2.5-4.5mol/L.
The preparation method of carbon fiber paper/Sodium Polyacrylate composite conducting gel film, comprises the following steps：
The reactant solution of polyacrylic acid sodium gel carries out polymerisation between two layers of carbon fiber paper is placed in after mixing, and obtains Plural gel piece, or by polymerize generation Sodium Polyacrylate gel film be placed in two layers of carbon fiber paper between, obtain plural gel piece； Plural gel piece infiltrates conductive ion solution, obtains composite conducting gel film after drying.
Preferably, the hydrogel is Sodium Polyacrylate hydrogel.
It is further preferred that the specific preparation method of carbon fiber paper/Sodium Polyacrylate composite conducting gel film, including it is as follows Step：
1) sodium acrylate monomers solution is prepared；
2) mixed solution of water-soluble cross-linked monomer and sodium peroxydisulfate is prepared；
3) application of vacuum after the solution in step 1) and step 2) is mixed；
4) mixed solution of application of vacuum to be poured into reaction vessel, the bottom of reaction vessel is covered with carbon fiber paper, and Tile carbon fiber paper in the upper surface of mixed solution；
5) polymerisation occurs for the mixed solution of step 4), obtains plural gel piece；
6) after the plural gel piece infiltration conductive ion solution, carbon fiber paper/Sodium Polyacrylate composite guide coagulation is obtained Film；
As long as not influenceing to prepare, above step is interchangeable.
Preferably, in step 1), sodium acrylate solution is mixed with by acrylic acid solution and sodium hydroxide solution.
It is further preferred that the mass fraction of the acrylic acid solution is 45-55%, the mass fraction of the sodium hydroxide For 20-30%.
Preferably, the mass ratio of acrylic acid, sodium hydroxide, N, N-2 NMAs and sodium peroxydisulfate is 100:45- 55:8-13:0.8-1.2.Sodium peroxydisulfate plays a part of initiator.
Preferably, in step 3), the vacuum of application of vacuum is 80kPa to 100kPa, and the time of application of vacuum is 6- 10h。
Application of vacuum can reduce the stomata in Sodium Polyacrylate gel film, because stomata can reduce conductance too much.
Preferably, in step 5), the temperature of polymerisation is 65-75 DEG C, and the time of polymerisation is 2-4h.
Preferably, in step 5), the surface of obtained plural gel piece is cleaned, further, uses alcohol pair The surface of plural gel piece is cleaned.
It is further preferred that in step 5), the plural gel piece after cleaning is dried, it is preferred that dry temperature For 55-65 DEG C, the dry time is 8-12h.
Preferably, in step 6), the conductive ion solution is sodium chloride solution, concentration 2.5-4.5mol/L.
A kind of preparation system of composite conducting gel film, including solution preparation device, polymerizing reactor, drying device and Infiltration apparatus, the preparation of reactant solution is carried out in solution preparation device；The mixed solution of reactant enters polymerizing reactor Generation polymerisation, hydrogel is generated, carbon fiber paper is provided with polymerizing reactor, realize the upper and lower surface difference of hydrogel With the bonding of carbon fiber paper, plural gel piece is obtained；After plural gel piece is dried in drying device, soaked into infiltration apparatus Moisten conductive ion solution, obtain composite conducting gel film.
Preferably, the preparation system also includes vacuum treatment installation, and mixed solution enters in vacuum treatment installation first After row application of vacuum, enter back into polymerizing reactor and polymerisation occurs.
The carbon fiber paper/Sodium Polyacrylate composite conducting gel film is as the conduction between defibrillation electrode and human skin The application of medium.
Beneficial effects of the present invention are：
1st, on the one hand the carbon fiber paper in composite conducting gel film of the invention can improve the mechanical strength of gel film, separately On the one hand it is electrically conductive, improve the electric conductivity of gel film jointly with the conductive ion in gel film.
2nd, the carbon fiber paper/Sodium Polyacrylate composite conducting gel film prepared, the advantages of nontoxic raw materials of use is pollution-free, degradable Green raw material, while raw material sources are extensive, and cost is more cheap, because it applies sodium chloride conductive ion, has to human skin Good compatibility, it can ensure that electrode current just as the conducting medium in defibrillation procedure between defibrillator and skin Often transmission.
3rd, the equipment that method of the invention uses is simple, and easy to operate, reaction temperature is relatively low (65 DEG C -75 DEG C), reaction production Thing processing is simple, and stable preparation process, production efficiency is high, suitable for mass production.
Embodiment
Below by specific embodiment, the invention will be further described.
Embodiment 1
A kind of preparation system of composite conducting gel film, including solution preparation device, vacuum treatment installation, polymerisation dress Put, drying device and infiltration apparatus, the preparation of reactant solution is carried out in solution preparation device；The reactant solution prepared passes through By vacuum treatment installation degasification, the mixed solution after degasification enters polymerizing reactor and occurs to gather the mixed solution being mixed to get Reaction is closed, hydrogel is generated, carbon fiber paper is provided with polymerizing reactor, realizes that the upper and lower surface of hydrogel is fine with carbon respectively The bonding of paper is tieed up, obtains plural gel piece；After plural gel piece is dried in drying device, infiltrated into infiltration apparatus conductive Solion, obtain composite conducting gel film.
A kind of preparation method of the composite conducting gel film of carbon fiber paper and Sodium Polyacrylate, comprises the following steps：
1) acrylic acid solution that mass concentration is 45% is taken, adds quality point into this acrylic acid solution under agitation Several 20% sodium hydroxide solutions, sodium acrylate solution is obtained after being well mixed；
2) N of acrylic monomers quality 0.1%, N-2 NMAs and acrylic monomers quality 1.2% mistake are taken Sodium sulphate is in 5ml water, ultrasonic dissolution 30min.
3) solution 1), 2) configured is placed in vacuum drying chamber, vacuumize process 6h is carried out under -80kpa.
4) by after two kinds of solution ultrasonic mixings after application of vacuum in 3), the culture dish for being equipped with a carbon fiber paper is poured into In, after being finished down mixed liquor, tiled a carbon fiber paper again on mixed solution surface, while polymerisation is carried out at a temperature of 70 DEG C 3h。
5) it is 90% alcohol washes surface by the gel film concentration having polymerize in 4), 8h is then dried at 60 DEG C.
6) after the gel film infiltration sodium chloride solution formed polymerisation in 5), carbon fiber/polypropylene acid is ultimately formed Sodium conductive hydrogel piece.
The structure of obtained carbon fiber/polypropylene acid sodium conductive hydrogel piece is：Including Sodium Polyacrylate gel film, first Carbon fiber paper and the second carbon fiber paper, Sodium Polyacrylate gel film is between the first carbon fiber paper and the second carbon fiber paper, structure Into laminated construction；Conductive ion solution is adsorbed with Sodium Polyacrylate gel film.
The defibrillator is 0.64ms/cm with the electrical conductivity of conduction electrocoagulation film.
Embodiment 2
A kind of preparation method of the composite conducting gel film of carbon fiber paper and Sodium Polyacrylate, comprises the following steps：
1) acrylic acid solution that mass concentration is 50% is taken, adds quality point into this acrylic acid solution under agitation Several 20% sodium hydroxide solutions, sodium acrylate solution is obtained after being well mixed；
2) N of acrylic monomers quality 0.1%, N-2 NMAs and acrylic monomers quality 1.2% mistake are taken Sodium sulphate is in 5ml water, ultrasonic dissolution 30min.
3) solution 1), 2) configured is placed in vacuum drying chamber, vacuumize process 6h is carried out under -80kpa.
4) by after two kinds of solution ultrasonic mixings after application of vacuum in 3), the culture dish for being equipped with a carbon fiber paper is poured into In, after being finished down mixed liquor, tiled a carbon fiber paper again on mixed solution surface, while polymerisation is carried out at a temperature of 70 DEG C 3h。
5) it is 90% alcohol washes surface by the gel film concentration having polymerize in 4), 10h is then dried at 60 DEG C.
6) after the gel film infiltration sodium chloride solution formed polymerisation in 5), carbon fiber/polypropylene acid is ultimately formed Sodium conductive hydrogel piece.
The defibrillator is 0.86ms/cm with the electrical conductivity of conduction electrocoagulation film.
Embodiment 3
A kind of preparation method of the composite conducting gel film of carbon fiber paper and Sodium Polyacrylate, comprises the following steps：
1) acrylic acid solution that mass concentration is 50% is taken, adds quality point into this acrylic acid solution under agitation Several 25% sodium hydroxide solutions, sodium acrylate solution is obtained after being well mixed；
2) N of acrylic monomers quality 0.15% is taken, N-2 NMAs and acrylic monomers quality 1.2% Sodium peroxydisulfate is in 5ml water, ultrasonic dissolution 30min.
3) solution 1), 2) configured is placed in vacuum drying chamber, vacuumize process 6h is carried out under -80kpa.
4) by after two kinds of solution ultrasonic mixings after application of vacuum in 3), the culture dish for being equipped with a carbon fiber paper is poured into In, after being finished down mixed liquor, tiled a carbon fiber paper again on mixed solution surface, while polymerisation is carried out at a temperature of 70 DEG C 3h。
5) it is 90% alcohol washes surface by the gel film concentration having polymerize in 4), 10h is then dried at 60 DEG C.
6) after the gel film infiltration sodium chloride solution formed polymerisation in 5), carbon fiber/polypropylene acid is ultimately formed Sodium conductive hydrogel piece.
The defibrillator is 1.22ms/cm with the electrical conductivity of conduction electrocoagulation film.
Embodiment 4
A kind of preparation method of the composite conducting gel film of carbon fiber paper and Sodium Polyacrylate, comprises the following steps：
1) acrylic acid solution that mass concentration is 50% is taken, adds quality point into this acrylic acid solution under agitation Several 25% sodium hydroxide solutions, sodium acrylate solution is obtained after being well mixed；
2) N of acrylic monomers quality 0.2%, N-2 NMAs and acrylic monomers quality 1.5% mistake are taken Sodium sulphate is in 5ml water, ultrasonic dissolution 30min.
3) solution 1), 2) configured is placed in vacuum drying chamber, vacuumize process 6h is carried out under -80kpa.
4) by after two kinds of solution ultrasonic mixings after application of vacuum in 3), the culture dish for being equipped with a carbon fiber paper is poured into In, after being finished down mixed liquor, tiled a carbon fiber paper again on mixed solution surface, while polymerisation is carried out at a temperature of 75 DEG C 3h。
5) it is 90% alcohol washes surface by the gel film concentration having polymerize in 4), 10h is then dried at 60 DEG C.
6) after the gel film infiltration sodium chloride solution formed polymerisation in 5), carbon fiber/polypropylene acid is ultimately formed Sodium conductive hydrogel piece.
The defibrillator is 0.92ms/cm with the electrical conductivity of conduction electrocoagulation film.
Although the above-mentioned embodiment to the present invention is described, the limitation not to invention protection domain, One of ordinary skill in the art should be understood that on the basis of technical scheme those skilled in the art need not pay The various modifications or deformation that creative work can be made are still within the scope of the present invention.

Claims (11)

  1. A kind of 1. composite conducting gel film of carbon fiber paper and Sodium Polyacrylate, it is characterised in that：Including polyacrylic acid sodium gel Piece, the first carbon fiber paper and the second carbon fiber paper, Sodium Polyacrylate gel film are located at the first carbon fiber paper and the second carbon fiber paper Between, form laminated construction；Conductive ion solution is adsorbed with Sodium Polyacrylate gel film；
    Its preparation method, comprise the following steps：
    The reactant solution of polyacrylic acid sodium gel carries out polymerisation between two layers of carbon fiber paper is placed in after mixing, and obtains compound Gel film, or by polymerize generation Sodium Polyacrylate gel film be placed in two layers of carbon fiber paper between, obtain plural gel piece；It is compound Gel film infiltrates conductive ion solution, obtains composite conducting gel film after drying.
  2. 2. the composite conducting gel film of carbon fiber paper according to claim 1 and Sodium Polyacrylate, it is characterised in that：It has Preparation comprises the following steps：
    1）Prepare sodium acrylate monomers solution；
    2）Prepare the mixed solution of water-soluble cross-linked monomer and sodium peroxydisulfate；
    3）By step 1）With step 2）In solution mixing after application of vacuum；
    4）The mixed solution of application of vacuum to be poured into reaction vessel, the bottom of reaction vessel is covered with carbon fiber paper, and mixed Close the upper surface tiling carbon fiber paper of solution；
    5）Step 4）Mixed solution occur polymerisation, obtain plural gel piece；
    6）After the plural gel piece infiltration conductive ion solution, carbon fiber paper/Sodium Polyacrylate composite conducting gel film is obtained；
    As long as not influenceing to prepare, above step is interchangeable.
  3. 3. the composite conducting gel film of carbon fiber paper according to claim 2 and Sodium Polyacrylate, it is characterised in that：Step 3）In, the vacuum of application of vacuum is 80kPa to 100kPa, and the time of application of vacuum is 6-10h.
  4. 4. the composite conducting gel film of carbon fiber paper according to claim 2 and Sodium Polyacrylate, it is characterised in that：Step 5）In, the surface of obtained plural gel piece is cleaned.
  5. 5. the composite conducting gel film of carbon fiber paper according to claim 4 and Sodium Polyacrylate, it is characterised in that：Use Alcohol cleans to the surface of plural gel piece.
  6. 6. the composite conducting gel film of carbon fiber paper according to claim 2 and Sodium Polyacrylate, it is characterised in that：Step 5）In, the plural gel piece after cleaning is dried.
  7. 7. the composite conducting gel film of carbon fiber paper according to claim 6 and Sodium Polyacrylate, it is characterised in that：Dry Temperature be 55-65 DEG C, the dry time is 8-12h.
  8. 8. the composite conducting gel film of carbon fiber paper according to claim 2 and Sodium Polyacrylate, it is characterised in that：Step 6）In, the conductive ion solution is sodium chloride solution, concentration 2.5-4.5mol/L.
  9. 9. the preparation system of the composite conducting gel film of any described carbon fiber papers of claim 1-8 and Sodium Polyacrylate, its It is characterised by：Including solution preparation device, polymerizing reactor, drying device and infiltration apparatus, carried out in solution preparation device The preparation of reactant solution；The mixed solution of reactant enters polymerizing reactor and polymerisation occurs, and generates hydrogel, polymerization Carbon fiber paper is provided with reaction unit, realizes the upper and lower surface of the hydrogel bonding with carbon fiber paper respectively, is obtained compound solidifying Film；After plural gel piece is dried in drying device, conductive ion solution is infiltrated into infiltration apparatus, obtains composite conducting Gel film.
  10. 10. preparation system according to claim 9, it is characterised in that：The preparation system also includes vacuum treatment installation, After mixed solution carries out application of vacuum first in vacuum treatment installation, enter back into polymerizing reactor and polymerisation occurs.
  11. 11. the composite conducting gel film of the carbon fiber paper and Sodium Polyacrylate described in claim 1 is as defibrillation electrode and human body The application of conducting medium between skin.
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