CN107501895A - A kind of preparation method of composite nanometer conductive material - Google Patents

A kind of preparation method of composite nanometer conductive material Download PDF

Info

Publication number
CN107501895A
CN107501895A CN201710843835.7A CN201710843835A CN107501895A CN 107501895 A CN107501895 A CN 107501895A CN 201710843835 A CN201710843835 A CN 201710843835A CN 107501895 A CN107501895 A CN 107501895A
Authority
CN
China
Prior art keywords
parts
minutes
hours
conductive material
distilled water
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710843835.7A
Other languages
Chinese (zh)
Inventor
原晋波
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201710843835.7A priority Critical patent/CN107501895A/en
Publication of CN107501895A publication Critical patent/CN107501895A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L71/00Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
    • C08L71/02Polyalkylene oxides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • C08K2003/162Calcium, strontium or barium halides, e.g. calcium, strontium or barium chloride
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/16Halogen-containing compounds
    • C08K2003/164Aluminum halide, e.g. aluminium chloride
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/001Conductive additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)

Abstract

The invention provides a kind of preparation method of composite nanometer conductive material, comprise the following steps:Stirring after copper chloride, alchlor, calcium chloride, ferric chloride (FeCl36H2O) and ethylene glycol ultrasound is added into anhydrous sodium acetate and polyethylene glycol;Add in polytetrafluoroethylene (PTFE) and reacted in kettle, washing and drying obtains product A;Nano zine oxide, polyoxyethylene sorbitan monoleate, Aerosol OT, lauroyl diethanolamine and distilled water are mixed, add product A, ultrasonic disperse;Stood after stopping stirring, add cocinic acid, phytic acid and pyrrole monomer, stirring reaction after cooling, filtration washing drying, obtain product B;Product B and distilled water are mixed, iron pentacarbonyl, piperidines and ammonium metavanadate is added, formic acid, stirring reaction, filtration washing drying is added under water-bath.Material easy processing shaping prepared by the preparation method of this composite nanometer conductive material, electric conductivity is splendid, all has potential application value in terms of electric transducer, solar cell, ultracapacitor.

Description

A kind of preparation method of composite nanometer conductive material
Technical field
The present invention relates to a kind of preparation method of composite nanometer conductive material.
Background technology
Nanometer technology is emerging in the last few years, has a kind of technology with broad prospects for development, at present to a certain degree On be used for the industries such as medicine, chemistry, electronic information and machinery.Nanometer technology refers to manufacture material with single atom, molecule Science and technology, research structure the size property of material and application in 0.1 to 100 nanometer range.And so-called nano material, refer to It is at least one-dimensional in nano-scale (0.1-100 nm) or by the material that they are formed as elementary cell in three dimensions, This is about as much as the yardstick that 10-100 atom is arranged closely together.Because its size is already close to the relevant length of electronics Degree, great changes will take place because strong relevant caused self-organizing causes property for its property, also, its yardstick is close to light Wavelength, has the special effects of large surface plus it, therefore its characteristic for being showed, such as fusing point, magnetic, optics, heat conduction, conduction Characteristic etc., the property often showed different from the material in integrality.At present, existing a variety of nano materials are closed Into such as nano semiconductor material and metal nano material.In recent years, nanometer conductive material is also included into nano materials research model Enclose, but nanometer conductive material processing is whard to control, the lattice structure not determined, therefore, it is also desirable to largely next pair of research It is controlled and improved.
The content of the invention
Technical problems to be solved:It is an object of the invention to provide a kind of preparation method of composite nanometer conductive material, institute The composite nanometer conductive material easy processing shaping of preparation, electric conductivity is splendid, in electric transducer, solar cell, ultracapacitor Aspect all has potential application value.
Technical scheme:A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:By 2-4 parts copper chloride, 1-3 parts alchlor, 1-2 parts calcium chloride, 1-2 parts ferric chloride (FeCl36H2O) and 80-100 parts Ethylene glycol is mixed, and 7-9 part nothings are added while stirring under rotating speed 200-400r/min with magnetic stirrer after ultrasonic 20-30 minutes Water sodium acetate and 2-3 part polyethylene glycol, continue to stir 30-40 minutes;
Step 2:Add in polytetrafluoroethylene (PTFE) in kettle, 7-9 hours are reacted at 220-240 DEG C, are entered respectively with distilled water and ethanol Row washing, is put into baking oven and dries, obtain product A;
Step 3:By 0.2-0.5 parts nano zine oxide, 0.3-0.7 parts Tween-80,0.2-0.4 part butanedioic acid di-isooctyls Sodium sulfonate, 0.1-0.3 parts lauroyl diethanolamine and 80-120 parts distilled water mix, and add product A, are put into Ultrasound Instrument Carry out ultrasonic disperse 2-3 hours;
Step 4:10-15 minutes are stood after stopping stirring, add 0.5-1 parts cocinic acid, 0.2-0.4 parts phytic acid and 1-2 part pyrroles Monomer is coughed up, is put into refrigerator, 5-10 minutes are cooled down at 0-5 DEG C of temperature, stirring reaction 2-3 hours after taking-up, filtering, are used respectively Distilled water and ethanol are washed, and are put into baking oven and are dried, and obtain product B;
Step 5:Product B and 20-30 part distilled water is mixed, carries out ultrasonic disperse, adds 1-2 parts iron pentacarbonyl, 0.1-0.2 parts Piperidines and 0.1-0.2 part ammonium metavanadates, water-bath at being 80-100 DEG C in temperature, add 2-5 part formic acid, 30-50 points of stirring reaction Clock;
Step 6:Continue at normal temperatures stirring reaction 2-3 hours, filtering, washed respectively with distilled water and ethanol, be put into baking Drying in case.
It is further preferred that ultrasonic time is 25 minutes, rotating speed 250-350r/min in step 1, mixing time is 35 points Clock.
It is further preferred that temperature is 230 DEG C in step 2, the reaction time is 8 hours.
It is further preferred that jitter time is 2.5 hours in step 3.
It is further preferred that temperature is 1-3 DEG C in step 4, cool time is 7-9 minutes, and the normal-temperature reaction time is 2.5 small When.
It is further preferred that bath temperature is 85-95 DEG C in step 5, the reaction time is 35-45 minutes.
It is further preferred that the stirring reaction time is 2.5 hours in step 6.
Beneficial effect:With the composite nanometer conductive material prepared by the present invention, particle diameter is between 5.5-5.7nm, easy processing Shaping, electric conductivity is splendid, and electrical conductivity reaches as high as 211S/cm, in terms of electric transducer, solar cell, ultracapacitor all With potential application value.
Embodiment
Embodiment 1
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:2 parts of copper chlorides, 1 part of alchlor, 1 part of calcium chloride, 1 part of ferric chloride (FeCl36H2O) and 80 parts of ethylene glycol are mixed, Ultrasound adds 7 parts of anhydrous sodium acetates and 2 parts of poly- second two with magnetic stirrer while stirring after 20 minutes under rotating speed 200r/min Alcohol, continue stirring 30 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7 hours at 220 DEG C, washed respectively with distilled water and ethanol, It is put into baking oven and dries, obtains product A;
Step 3:By 0.2 part of nano zine oxide, 0.3 part of Tween-80,0.2 part of Aerosol OT, 0.1 part Lauroyl diethanolamine and 80 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 2 hours;
Step 4:10 minutes are stood after stopping stirring, 0.5 part of cocinic acid, 0.2 part of phytic acid and 1 part of pyrrole monomer is added, is put into In refrigerator, cool down 5 minutes, stirring reaction 2 hours after taking-up, filtering, washed respectively with distilled water and ethanol at 0 DEG C of temperature Wash, be put into baking oven and dry, obtain product B;
Step 5:Product B and 20 parts of distilled water are mixed, carry out ultrasonic disperse, adds 1 part of iron pentacarbonyl, 0.1 part of piperidines and 0.1 Part ammonium metavanadate, water-bath at being 80 DEG C in temperature, adds 2 parts of formic acid, stirring reaction 30 minutes;
Step 6:Continue stirring reaction at normal temperatures 2 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven Middle drying.
Embodiment 2
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:By 2.5 parts of copper chlorides, 1.5 parts of alchlors, 1.5 parts of calcium chloride, 1.5 parts of ferric chloride (FeCl36H2O)s and 85 parts of second two Alcohol mixes, and ultrasound adds 8 parts of anhydrous sodium acetates and 2.5 with magnetic stirrer while stirring after 25 minutes under rotating speed 250r/min Part polyethylene glycol, continues stirring 35 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7.5 hours at 225 DEG C, washed respectively with distilled water and ethanol Wash, be put into baking oven and dry, obtain product A;
Step 3:By 0.3 part of nano zine oxide, 0.4 part of Tween-80,0.25 part of Aerosol OT, 0.15 Part lauroyl diethanolamine and 90 parts of distilled water mix, and add product A, and it is small to be put into progress ultrasonic disperse 2.5 in Ultrasound Instrument When;
Step 4:11 minutes are stood after stopping stirring, 0.6 part of cocinic acid, 0.25 part of phytic acid and 1.5 parts of pyrrole monomers is added, puts Enter in refrigerator, cooled down 6 minutes at 1 DEG C of temperature, stirring reaction 2.5 hours after taking-up, filtering, entered respectively with distilled water and ethanol Row washing, is put into baking oven and dries, obtain product B;
Step 5:Product B and 25 parts of distilled water are mixed, carry out ultrasonic disperse, add 1.2 parts of iron pentacarbonyls, 0.15 part of piperidines and 0.12 part of ammonium metavanadate, water-bath at being 90 DEG C in temperature, adds 3 parts of formic acid, stirring reaction 35 minutes;
Step 6:Continue stirring reaction at normal temperatures 2.5 hours, filtering, washed respectively with distilled water and ethanol, be put into baking Drying in case.
Embodiment 3
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:3 parts of copper chlorides, 2 parts of alchlors, 1.5 parts of calcium chloride, 1.5 parts of ferric chloride (FeCl36H2O)s and 90 parts of ethylene glycol are mixed Close, ultrasound adds 8 parts of anhydrous sodium acetates while stirring under rotating speed 300r/min with magnetic stirrer after 25 minutes and 2.5 parts poly- Ethylene glycol, continue stirring 35 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 8 hours at 230 DEG C, washed respectively with distilled water and ethanol, It is put into baking oven and dries, obtains product A;
Step 3:By 0.35 part of nano zine oxide, 0.5 part of Tween-80,0.3 part of Aerosol OT, 0.2 part Lauroyl diethanolamine and 100 parts of distilled water mix, and add product A, and it is small to be put into progress ultrasonic disperse 2.5 in Ultrasound Instrument When;
Step 4:13 minutes are stood after stopping stirring, 0.7 part of cocinic acid, 0.3 part of phytic acid and 1.5 parts of pyrrole monomers is added, puts Enter in refrigerator, cooled down 7 minutes at 3 DEG C of temperature, stirring reaction 2.5 hours after taking-up, filtering, entered respectively with distilled water and ethanol Row washing, is put into baking oven and dries, obtain product B;
Step 5:Product B and 25 parts of distilled water are mixed, carry out ultrasonic disperse, add 1.5 parts of iron pentacarbonyls, 0.15 part of piperidines and 0.15 part of ammonium metavanadate, water-bath at being 90 DEG C in temperature, adds 3.5 parts of formic acid, stirring reaction 40 minutes;
Step 6:Continue stirring reaction at normal temperatures 2.5 hours, filtering, washed respectively with distilled water and ethanol, be put into baking Drying in case.
Embodiment 4
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:By 3.5 parts of copper chlorides, 2.5 parts of alchlors, 1.5 parts of calcium chloride, 1.5 parts of ferric chloride (FeCl36H2O)s and 95 parts of second two Alcohol mixes, and ultrasound adds 8 parts of anhydrous sodium acetates and 2.5 with magnetic stirrer while stirring after 25 minutes under rotating speed 350r/min Part polyethylene glycol, continues stirring 35 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 8.5 hours at 235 DEG C, washed respectively with distilled water and ethanol Wash, be put into baking oven and dry, obtain product A;
Step 3:By 0.4 part of nano zine oxide, 0.6 part of Tween-80,0.35 part of Aerosol OT, 0.25 Part lauroyl diethanolamine and 110 parts of distilled water mix, and add product A, and it is small to be put into progress ultrasonic disperse 2.5 in Ultrasound Instrument When;
Step 4:14 minutes are stood after stopping stirring, 0.9 part of cocinic acid, 0.35 part of phytic acid and 1.5 parts of pyrrole monomers is added, puts Enter in refrigerator, cooled down 9 minutes at 4 DEG C of temperature, stirring reaction 2.5 hours after taking-up, filtering, entered respectively with distilled water and ethanol Row washing, is put into baking oven and dries, obtain product B;
Step 5:Product B and 25 parts of distilled water are mixed, carry out ultrasonic disperse, add 1.5 parts of iron pentacarbonyls, 0.15 part of piperidines and 0.15 part of ammonium metavanadate, water-bath at being 95 DEG C in temperature, adds 4 parts of formic acid, stirring reaction 45 minutes;
Step 6:Continue stirring reaction at normal temperatures 2.5 hours, filtering, washed respectively with distilled water and ethanol, be put into baking Drying in case.
Embodiment 5
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:4 parts of copper chlorides, 3 parts of alchlors, 2 parts of calcium chloride, 2 parts of ferric chloride (FeCl36H2O)s and 100 parts of ethylene glycol are mixed, Ultrasound adds 9 parts of anhydrous sodium acetates and 3 parts of poly- second two with magnetic stirrer while stirring after 30 minutes under rotating speed 400r/min Alcohol, continue stirring 40 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 9 hours at 240 DEG C, washed respectively with distilled water and ethanol, It is put into baking oven and dries, obtains product A;
Step 3:By 0.5 part of nano zine oxide, 0.7 part of Tween-80,0.4 part of Aerosol OT, 0.3 part Lauroyl diethanolamine and 120 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 3 hours;
Step 4:15 minutes are stood after stopping stirring, 1 part of cocinic acid, 0.4 part of phytic acid and 2 parts of pyrrole monomers is added, is put into ice In case, cool down 10 minutes, stirring reaction 3 hours after taking-up, filtering, washed respectively with distilled water and ethanol at 5 DEG C of temperature Wash, be put into baking oven and dry, obtain product B;
Step 5:Product B and 30 parts of distilled water are mixed, carry out ultrasonic disperse, adds 2 parts of iron pentacarbonyls, 0.2 part of piperidines and 0.2 Part ammonium metavanadate, water-bath at being 100 DEG C in temperature, adds 2-5 part formic acid, stirring reaction 50 minutes;
Step 6:Continue stirring reaction at normal temperatures 3 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven Middle drying.
Comparative example 1
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:2 parts of copper chlorides, 1 part of alchlor, 1 part of calcium chloride, 1 part of ferric chloride (FeCl36H2O) and 80 parts of ethylene glycol are mixed, Ultrasound adds 7 parts of anhydrous sodium acetates and 2 parts of poly- second two with magnetic stirrer while stirring after 20 minutes under rotating speed 200r/min Alcohol, continue stirring 30 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7 hours at 220 DEG C, washed respectively with distilled water and ethanol, It is put into baking oven and dries, obtains product A;
Step 3:By 0.2 part of nano zine oxide, 0.3 part of Tween-80,0.2 part of Aerosol OT, 0.1 part Lauroyl diethanolamine and 80 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 2 hours;
Step 4:Stands 10 minutes after stopping stirring, add 1 part of pyrrole monomer, be put into refrigerator, 5 points of the cooling at 0 DEG C of temperature Clock, stirring reaction 2 hours after taking-up, filtering, washed respectively with distilled water and ethanol, be put into baking oven and dry, obtain product B;
Step 5:Product B and 20 parts of distilled water are mixed, carry out ultrasonic disperse, adds 1 part of iron pentacarbonyl, 0.1 part of piperidines and 0.1 Part ammonium metavanadate, water-bath at being 80 DEG C in temperature, adds 2 parts of formic acid, stirring reaction 30 minutes;
Step 6:Continue stirring reaction at normal temperatures 2 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven Middle drying.
Comparative example 2
A kind of preparation method of composite nanometer conductive material, comprises the following steps:
Step 1:3 parts of copper chlorides, 2 parts of ferric chloride (FeCl36H2O)s and 80 parts of ethylene glycol are mixed, ultrasound uses magnetic agitation after 20 minutes Machine adds 7 parts of anhydrous sodium acetates and 2 parts of polyethylene glycol while stirring under rotating speed 200r/min, continues stirring 30 minutes;
Step 2:In addition polytetrafluoroethylene (PTFE) in kettle, react 7 hours at 220 DEG C, washed respectively with distilled water and ethanol, It is put into baking oven and dries, obtains product A;
Step 3:By 0.2 part of nano zine oxide, 0.3 part of Tween-80,0.2 part of Aerosol OT, 0.1 part Lauroyl diethanolamine and 80 parts of distilled water mix, and add product A, are put into Ultrasound Instrument and carry out ultrasonic disperse 2 hours;
Step 4:10 minutes are stood after stopping stirring, 0.5 part of cocinic acid, 0.2 part of phytic acid and 1 part of pyrrole monomer is added, is put into In refrigerator, cool down 5 minutes, stirring reaction 2 hours after taking-up, filtering, washed respectively with distilled water and ethanol at 0 DEG C of temperature Wash, be put into baking oven and dry, obtain product B;
Step 5:Product B and 20 parts of distilled water are mixed, carry out ultrasonic disperse, adds 1 part of iron pentacarbonyl, 0.1 part of piperidines and 0.1 Part ammonium metavanadate, water-bath at being 80 DEG C in temperature, adds 2 parts of formic acid, stirring reaction 30 minutes;
Step 6:Continue stirring reaction at normal temperatures 2 hours, filtering, washed respectively with distilled water and ethanol, be put into baking oven Middle drying.
Each embodiment is compared with comparative example, comparing result is as shown in the table, it may be seen that prepared by the present invention Material particle size is between 5.5-5.7nm, and easy processing shaping, electric conductivity is splendid, and electrical conductivity reaches as high as 211S/cm, in fax sense All there is potential application value in terms of device, solar cell, ultracapacitor.
The partial properties index of the composite nanometer conductive material of table 1
Name of product Material particle size(nm) Electrical conductivity(S/cm)
Embodiment 1 5.5 205
Embodiment 2 5.5 208
Embodiment 3 5.7 209
Embodiment 4 5.6 211
Embodiment 5 5.5 208
Comparative example 1 5.5 201
Comparative example 2 5.8 189

Claims (7)

  1. A kind of 1. preparation method of composite nanometer conductive material, it is characterised in that:Comprise the following steps:
    Step 1:By 2-4 parts copper chloride, 1-3 parts alchlor, 1-2 parts calcium chloride, 1-2 parts ferric chloride (FeCl36H2O) and 80-100 parts Ethylene glycol is mixed, and 7-9 part nothings are added while stirring under rotating speed 200-400r/min with magnetic stirrer after ultrasonic 20-30 minutes Water sodium acetate and 2-3 part polyethylene glycol, continue to stir 30-40 minutes;
    Step 2:Add in polytetrafluoroethylene (PTFE) in kettle, 7-9 hours are reacted at 220-240 DEG C, are entered respectively with distilled water and ethanol Row washing, is put into baking oven and dries, obtain product A;
    Step 3:By 0.2-0.5 parts nano zine oxide, 0.3-0.7 parts Tween-80,0.2-0.4 part butanedioic acid di-isooctyls Sodium sulfonate, 0.1-0.3 parts lauroyl diethanolamine and 80-120 parts distilled water mix, and add product A, are put into Ultrasound Instrument Carry out ultrasonic disperse 2-3 hours;
    Step 4:10-15 minutes are stood after stopping stirring, add 0.5-1 parts cocinic acid, 0.2-0.4 parts phytic acid and 1-2 part pyrroles Monomer is coughed up, is put into refrigerator, 5-10 minutes are cooled down at 0-5 DEG C of temperature, stirring reaction 2-3 hours after taking-up, filtering, are used respectively Distilled water and ethanol are washed, and are put into baking oven and are dried, and obtain product B;
    Step 5:Product B and 20-30 part distilled water is mixed, carries out ultrasonic disperse, adds 1-2 parts iron pentacarbonyl, 0.1-0.2 parts Piperidines and 0.1-0.2 part ammonium metavanadates, water-bath at being 80-100 DEG C in temperature, add 2-5 part formic acid, 30-50 points of stirring reaction Clock;
    Step 6:Continue at normal temperatures stirring reaction 2-3 hours, filtering, washed respectively with distilled water and ethanol, be put into baking Drying in case.
  2. A kind of 2. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 1 Middle ultrasonic time is 25 minutes, rotating speed 250-350r/min, and mixing time is 35 minutes.
  3. A kind of 3. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 2 Middle temperature is 230 DEG C, and the reaction time is 8 hours.
  4. A kind of 4. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 3 Middle jitter time is 2.5 hours.
  5. A kind of 5. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 4 Middle temperature is 1-3 DEG C, and cool time is 7-9 minutes, and the normal-temperature reaction time is 2.5 hours.
  6. A kind of 6. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 5 Middle bath temperature is 85-95 DEG C, and the reaction time is 35-45 minutes.
  7. A kind of 7. preparation method of composite nanometer conductive material according to claim 1, it is characterised in that:The step 6 The middle stirring reaction time is 2.5 hours.
CN201710843835.7A 2017-09-19 2017-09-19 A kind of preparation method of composite nanometer conductive material Pending CN107501895A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710843835.7A CN107501895A (en) 2017-09-19 2017-09-19 A kind of preparation method of composite nanometer conductive material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710843835.7A CN107501895A (en) 2017-09-19 2017-09-19 A kind of preparation method of composite nanometer conductive material

Publications (1)

Publication Number Publication Date
CN107501895A true CN107501895A (en) 2017-12-22

Family

ID=60697750

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710843835.7A Pending CN107501895A (en) 2017-09-19 2017-09-19 A kind of preparation method of composite nanometer conductive material

Country Status (1)

Country Link
CN (1) CN107501895A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102161764A (en) * 2011-02-25 2011-08-24 东华大学 Method for preparing cobalt-zinc ferrite/polypyrrole nano composite material
CN105632586A (en) * 2016-03-22 2016-06-01 苏州捷德瑞精密机械有限公司 Nano conductive composite material and preparation method therefor
CN106340401A (en) * 2016-11-28 2017-01-18 中物院成都科学技术发展中心 Preparing method of composite electrode material and application thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102161764A (en) * 2011-02-25 2011-08-24 东华大学 Method for preparing cobalt-zinc ferrite/polypyrrole nano composite material
CN105632586A (en) * 2016-03-22 2016-06-01 苏州捷德瑞精密机械有限公司 Nano conductive composite material and preparation method therefor
CN106340401A (en) * 2016-11-28 2017-01-18 中物院成都科学技术发展中心 Preparing method of composite electrode material and application thereof

Similar Documents

Publication Publication Date Title
CN102993749B (en) A kind of nanometer Al 2o 3the corona-resistant polyimide film of compound
KR101003156B1 (en) Method to produce aqueous graphene solution and aqueous conductive polymer solution
CN101798462A (en) Graphene/conductive polymer composite film and preparation method thereof
CN105838086B (en) Preparation method of sulfonated carbon nanotube grafted hydroxylated polyether-ether-ketone/polyether-ether-ketone composite material
CN104313872A (en) Preparation method of graphene/polyaniline covalent binding conductive fabric
CN103224705A (en) Nano-modified polyimide composite film and preparation method thereof
CN106751587B (en) graphene 3D printing material and preparation method thereof
CN105153620A (en) Modified polypropylene/hyper branched polyimide insulated alloy material and preparation method thereof
CN108440740A (en) It a kind of reversible selfreparing epoxy resin and its prepares and recycling remodeling procedure
CN105085915B (en) A kind of high dielectric polyimides/carbon nano tube compound material and preparation method thereof
CN104774454B (en) A kind of high temperature resistant nylon PA66T materials and preparation method thereof
CN108864622A (en) A kind of preparation method of polymer-based dielectric composite material
CN101891936B (en) Preparation method of composite material based on epoxy resin and phosphazene nanotubes
CN107799204A (en) A kind of touch-screen graphene conductive film and preparation method thereof
CN103752815B (en) A kind of different-shape one-dimensional silver/manganese oxide composite preparation method and application thereof
CN105086301A (en) High-thermal-conductivity PTFE pipe for thermal power heat exchanger
CN107501895A (en) A kind of preparation method of composite nanometer conductive material
CN104292456A (en) Method for preparing polyaniline/graphene/ferroferric oxide composite material
CN112694750A (en) BT resin composite material containing nano MOFs and preparation method thereof
CN105802133A (en) Preparation method of graphene-based epoxy resin composite thermal interface material
JP2015034282A (en) Composite material for circuit board production, and circuit board ingredient material produced using the same
CN106221082A (en) A kind of composite of Gemini surface active modified calcium carbonate filled polytetrafluoroethylene and preparation method thereof
CN112852287A (en) Preparation method of nano silicon carbide loaded reduced graphene oxide compound modified thermosetting polyimide wear-resistant coating
CN105038228A (en) Polyimide high-dielectric composite film mixed with nano-boron carbide-loaded graphene and used for capacitor and preparation method thereof
CN105632586B (en) A kind of conductive nano composites and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20171222

WD01 Invention patent application deemed withdrawn after publication