CN106276867A - The photoelectric modified graphene of a kind of enhancing - Google Patents
The photoelectric modified graphene of a kind of enhancing Download PDFInfo
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- CN106276867A CN106276867A CN201610573000.XA CN201610573000A CN106276867A CN 106276867 A CN106276867 A CN 106276867A CN 201610573000 A CN201610573000 A CN 201610573000A CN 106276867 A CN106276867 A CN 106276867A
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- modified graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The invention discloses the photoelectric modified graphene of a kind of enhancing, it is characterized in that, its formula is as follows: native graphite 80 100 parts, strong oxidizer 10 15 parts, the first dispersant 37 parts, the second dispersant 6 11 parts, the first modifying agent 10 20 parts, the second modifying agent 20 35 parts, penetrating agent 37 parts, silicones 10 15 parts, metal-oxide 15 25 parts, levelling agent 17 parts, Polyethylene Glycol 20 28 parts.The present invention uses method modified inside and outside multilamellar, solves the problem reunited in materials application.
Description
Technical field
The invention belongs to technical field of macromolecules, be specifically related to the photoelectric modified graphene of a kind of enhancing.
Background technology
Graphene itself is prepared by graphite, and theoretical specific capacity is but 2 times of graphite, (graphite 372mAhg-1, Graphene
744 mAhg-1).Graphene itself is the thinnest, wraps up other compounds and forms complex, it is possible to improves application further.But stone
Ink alkene is easily reunited, and causes Graphene dispersive property to be in a solvent deteriorated, irreversible reunion occurs, cause graphene layer thickness to increase
Add.For this problem, Graphene is carried out multi-level modification, the problem solving to reunite in materials application.
Summary of the invention
It is an object of the invention to provide the photoelectric modified graphene of a kind of enhancing, the present invention uses inside and outside multilamellar modified
Method, solve in materials application reunite problem.
The photoelectric modified graphene of a kind of enhancing, its formula is as follows: native graphite 80-100 part, strong oxidizer 10-
15 parts, first dispersant 3-7 part, second dispersant 6-11 part, first modifying agent 10-20 part, second modifying agent 20-35 part, ooze
Agent 3-7 part, silicones 10-15 part, metal-oxide 15-25 part, levelling agent 1-7 part, Polyethylene Glycol 20-28 part thoroughly.
Described strong oxidizer uses potassium permanganate or potassium dichromate.
Described first dispersant uses polyvinylpyrrolidone, and described polyvinylpyrrolidone uses K90 model.
Described second dispersant uses kayexalate or dodecylbenzene sodium sulfonate.
Described first modifying agent uses 18-amine..
Described second modifying agent uses quaternary ammonium salt, and described quaternary ammonium salt includes Dodecyl trimethyl ammonium chloride, myristyl
At least one in trimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyl trimethyl ammonium chloride.
Described penetrating agent uses fatty alcohol-polyoxyethylene ether.
Described silicones uses organic siliconresin, uses methyl phenyl silicone resin, methyl silicon resin, low phenyl methyl silicon tree
One in fat or epoxy modified silicone resin.
Described metal-oxide uses zinc oxide or titanium dioxide.
A kind of preparation method strengthening photoelectric modified graphene, its step is as follows:
Step 1, proportionally weighs raw material；
Step 2, native graphite pulverizes, and pulverized particles is not more than 100 microns, and uses ethanol water to be carried out, low
Temperature is dried and is obtained powdered graphite；Ethanol content in described ethanol water is 20-50%, and oven drying at low temperature temperature is 50-60 DEG C；
Step 3, is added to the water powdered graphite with strong oxidizer, the first dispersant, carries out low-temperature heat, boil altogether, the coldest
Obtain graphene oxide serosity the most afterwards；Low-temperature heat temperature is 60-70 DEG C, and heat time heating time is 30-50min；
Step 4, carries out neutral cleaning, until in neutrality, being configured to graphene aqueous solution after drying by graphene oxide serosity；Institute
Stating drying temperature and be 80-100 DEG C, drying time is 20-30min；
Step 5, adds the first modifying agent, penetrating agent, the second dispersant in graphene aqueous solution, carries out water-bath backflow, obtain
Deep layer modified graphene solution；Described bath temperature is 90-105 DEG C, and return time is 60-120min；
Step 6, after carrying out deep layer modified graphene solution filtering cleaning, dries and obtains deep layer modified graphene powder body；
Step 7, puts in ethanol solution by deep layer modified graphene powder body, adds the second modifying agent, acid solution, ultrasonic resonance,
Clean to neutral after filtration, after drying, i.e. can get modified graphene powder body；Described supersonic frequency is 10-15MHz, described ultrasonic
Time is 20-35min；
Step 8, steams after modified graphene powder body, silicones, metal-oxide, levelling agent, Polyethylene Glycol mix and blend
Send to be formed thick, then carry out high temperature sintering, i.e. can get modified graphene material；Described evaporating temperature is 100-110
DEG C, high temperature sintering temperature is 300-500 DEG C, sintering time 300-480min.
Compared with prior art, the method have the advantages that
1, the present invention uses multiple dispersant to match with modifying agent to be modified, and has solution Graphene agglomeration traits, molten
Good dispersion in agent.
2, the present invention use silicones as the junctional complex of metal-oxide Yu graphene powder, can not only be after sintering
Element silicon in connection, has raising Graphene electron transfer effect, can increase metal-oxide and graphene powder simultaneously
Connectivity.
3, the present invention uses the mode that multilamellar is modified, it is possible to be greatly increased modified effect, it is possible to ensure the inside and outside of Graphene
Modifying function, uses metal-oxide to have the function well stopping hole transport electronics simultaneously, can effectively stop photoproduction
Being combined of electron-hole, and then improve photoelectric transformation efficiency, considerably increase photoelectric effect.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further:
Embodiment 1
A kind of strengthening photoelectric modified graphene, its formula is as follows: native graphite 80 parts, strong oxidizer 10 parts, first point
Powder 3 parts, the second dispersant 6 parts, the first modifying agent 10 parts, the second modifying agent 20 parts, penetrating agent 3 parts, silicones 10 parts, metal
Oxide 15 parts, levelling agent 1 part, Polyethylene Glycol 20 parts.
Described strong oxidizer uses potassium permanganate.
Described first dispersant uses polyvinylpyrrolidone, and described polyvinylpyrrolidone uses K90 model.
Described second dispersant uses kayexalate.
Described first modifying agent uses 18-amine..
Described second modifying agent uses quaternary ammonium salt, and described quaternary ammonium salt includes Dodecyl trimethyl ammonium chloride.
Described penetrating agent uses fatty alcohol-polyoxyethylene ether.
Described silicones uses organic siliconresin, uses methyl phenyl silicone resin.
Described metal-oxide uses zinc oxide.
A kind of preparation method strengthening photoelectric modified graphene, its step is as follows:
Step 1, proportionally weighs raw material；
Step 2, native graphite pulverizes, pulverized particles 100 microns, and uses ethanol water to be carried out, oven drying at low temperature
Obtain powdered graphite；Ethanol content in described ethanol water is 20%, and oven drying at low temperature temperature is 50 DEG C；
Step 3, is added to the water powdered graphite with strong oxidizer, the first dispersant, carries out low-temperature heat, boil altogether, the coldest
Obtain graphene oxide serosity the most afterwards；Low-temperature heat temperature is 60 DEG C, and heat time heating time is 30min；
Step 4, carries out neutral cleaning, until in neutrality, being configured to graphene aqueous solution after drying by graphene oxide serosity；Institute
Stating drying temperature is 80 DEG C, and drying time is 20min；
Step 5, adds the first modifying agent, penetrating agent, the second dispersant in graphene aqueous solution, carries out water-bath backflow, obtain
Deep layer modified graphene solution；Described bath temperature is 90 DEG C, and return time is 60min；
Step 6, after carrying out deep layer modified graphene solution filtering cleaning, dries and obtains deep layer modified graphene powder body；
Step 7, puts in ethanol solution by deep layer modified graphene powder body, adds the second modifying agent, acid solution, ultrasonic resonance,
Clean to neutral after filtration, after drying, i.e. can get modified graphene powder body；Described supersonic frequency is 10MHz, described ultrasonic time
Between be 20min；
Step 8, steams after modified graphene powder body, silicones, metal-oxide, levelling agent, Polyethylene Glycol mix and blend
Send to be formed thick, then carry out high temperature sintering, i.e. can get modified graphene material；Described evaporating temperature is 100 DEG C, high
Temperature sintering temperature is 300 DEG C, sintering time 300min.
Embodiment 2
A kind of strengthening photoelectric modified graphene, its formula is as follows: native graphite 100 parts, strong oxidizer 15 parts, first point
Powder 7 parts, the second dispersant 11 parts, the first modifying agent 20 parts, the second modifying agent 35 parts, penetrating agent 7 parts, silicones 15 parts, gold
Belong to oxide 25 parts, levelling agent 7 parts, Polyethylene Glycol 28 parts.
Described strong oxidizer uses potassium dichromate.
Described first dispersant uses polyvinylpyrrolidone, and described polyvinylpyrrolidone uses K90 model.
Described second dispersant uses dodecylbenzene sodium sulfonate.
Described first modifying agent uses 18-amine..
Described second modifying agent uses quaternary ammonium salt, and described quaternary ammonium salt includes tetradecyl trimethyl ammonium chloride.
Described penetrating agent uses fatty alcohol-polyoxyethylene ether.
Described silicones uses organic siliconresin, uses methyl silicon resin.
Described metal-oxide uses titanium dioxide.
A kind of preparation method strengthening photoelectric modified graphene, its step is as follows:
Step 1, proportionally weighs raw material；
Step 2, native graphite pulverizes, pulverized particles 10 microns, and uses ethanol water to be carried out, and oven drying at low temperature obtains
To powdered graphite；Ethanol content in described ethanol water is 50%, and oven drying at low temperature temperature is 60 DEG C；
Step 3, is added to the water powdered graphite with strong oxidizer, the first dispersant, carries out low-temperature heat, boil altogether, the coldest
Obtain graphene oxide serosity the most afterwards；Low-temperature heat temperature is 70 DEG C, and heat time heating time is 50min；
Step 4, carries out neutral cleaning, until in neutrality, being configured to graphene aqueous solution after drying by graphene oxide serosity；Institute
Stating drying temperature is 100 DEG C, and drying time is 30min；
Step 5, adds the first modifying agent, penetrating agent, the second dispersant in graphene aqueous solution, carries out water-bath backflow, obtain
Deep layer modified graphene solution；Described bath temperature is 105 DEG C, and return time is 120min；
Step 6, after carrying out deep layer modified graphene solution filtering cleaning, dries and obtains deep layer modified graphene powder body；
Step 7, puts in ethanol solution by deep layer modified graphene powder body, adds the second modifying agent, acid solution, ultrasonic resonance,
Clean to neutral after filtration, after drying, i.e. can get modified graphene powder body；Described supersonic frequency is 15MHz, described ultrasonic time
Between be 35min；
Step 8, steams after modified graphene powder body, silicones, metal-oxide, levelling agent, Polyethylene Glycol mix and blend
Send to be formed thick, then carry out high temperature sintering, i.e. can get modified graphene material；Described evaporating temperature is 110 DEG C, high
Temperature sintering temperature is 500 DEG C, sintering time 480min.
Embodiment 3
A kind of strengthening photoelectric modified graphene, its formula is as follows: native graphite 90 parts, strong oxidizer 13 parts, first point
Powder 5 parts, the second dispersant 9 parts, the first modifying agent 15 parts, the second modifying agent 27 parts, penetrating agent 5 parts, silicones 12 parts, metal
Oxide 20 parts, levelling agent 4 parts, Polyethylene Glycol 24 parts.
Described strong oxidizer uses potassium permanganate.
Described first dispersant uses polyvinylpyrrolidone, and described polyvinylpyrrolidone uses K90 model.
Described second dispersant uses kayexalate.
Described first modifying agent uses 18-amine..
Described second modifying agent uses quaternary ammonium salt, and described quaternary ammonium salt includes cetyl trimethylammonium bromide.
Described penetrating agent uses fatty alcohol-polyoxyethylene ether.
Described silicones uses organic siliconresin, uses epoxy modified silicone resin.
Described metal-oxide uses zinc oxide.
A kind of preparation method strengthening photoelectric modified graphene, its step is as follows:
Step 1, proportionally weighs raw material；
Step 2, native graphite pulverizes, pulverized particles 80 microns, and uses ethanol water to be carried out, and oven drying at low temperature obtains
To powdered graphite；Ethanol content in described ethanol water is 35%, and oven drying at low temperature temperature is 55 DEG C；
Step 3, is added to the water powdered graphite with strong oxidizer, the first dispersant, carries out low-temperature heat, boil altogether, the coldest
Obtain graphene oxide serosity the most afterwards；Low-temperature heat temperature is 65 DEG C, and heat time heating time is 40min；
Step 4, carries out neutral cleaning, until in neutrality, being configured to graphene aqueous solution after drying by graphene oxide serosity；Institute
Stating drying temperature is 90 DEG C, and drying time is 25min；
Step 5, adds the first modifying agent, penetrating agent, the second dispersant in graphene aqueous solution, carries out water-bath backflow, obtain
Deep layer modified graphene solution；Described bath temperature is 97 DEG C, and return time is 100min；
Step 6, after carrying out deep layer modified graphene solution filtering cleaning, dries and obtains deep layer modified graphene powder body；
Step 7, puts in ethanol solution by deep layer modified graphene powder body, adds the second modifying agent, acid solution, ultrasonic resonance,
Clean to neutral after filtration, after drying, i.e. can get modified graphene powder body；Described supersonic frequency is 12MHz, described ultrasonic time
Between be 25min；
Step 8, steams after modified graphene powder body, silicones, metal-oxide, levelling agent, Polyethylene Glycol mix and blend
Send to be formed thick, then carry out high temperature sintering, i.e. can get modified graphene material；Described evaporating temperature is 105 DEG C, high
Temperature sintering temperature is 400 DEG C, sintering time 390min.
The foregoing is only one embodiment of the invention, be not limiting as the present invention, all employing equivalents or equivalent transformation
The technical scheme that obtained of mode, all fall within protection scope of the present invention.
Claims (10)
1. one kind strengthens photoelectric modified graphene, it is characterised in that its formula is as follows: native graphite 80-100 part, strong
Oxidant 10-15 part, first dispersant 3-7 part, second dispersant 6-11 part, first modifying agent 10-20 part, the second modifying agent
20-35 part, penetrating agent 3-7 part, silicones 10-15 part, metal-oxide 15-25 part, levelling agent 1-7 part, Polyethylene Glycol 20-28
Part.
2. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described Strong oxdiative
Agent uses potassium permanganate or potassium dichromate.
3. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described first point
Powder uses polyvinylpyrrolidone, and described polyvinylpyrrolidone uses K90 model.
4. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described second point
Powder uses kayexalate or dodecylbenzene sodium sulfonate.
5. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described first changes
Property agent use 18-amine..
6. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described second changes
Property agent use quaternary ammonium salt, described quaternary ammonium salt includes Dodecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride, hexadecane
At least one in base trimethylammonium bromide, octadecyl trimethyl ammonium chloride.
7. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described penetrating agent
Use fatty alcohol-polyoxyethylene ether.
8. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described silicones
Use organic siliconresin, use methyl phenyl silicone resin, methyl silicon resin, low phenyl methyl silicones or epoxy modified silicone
One in resin.
9. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that described metal oxygen
Compound uses zinc oxide or titanium dioxide.
10. strengthen photoelectric modified graphene according to the one described in claims 1, it is characterised in that modified graphite
The preparation method of alkene, its step is as follows:
Step 1, proportionally weighs raw material；
Step 2, native graphite pulverizes, and pulverized particles is not more than 100 microns, and uses ethanol water to be carried out, low
Temperature is dried and is obtained powdered graphite；Ethanol content in described ethanol water is 20-50%, and oven drying at low temperature temperature is 50-60 DEG C；
Step 3, is added to the water powdered graphite with strong oxidizer, the first dispersant, carries out low-temperature heat, boil altogether, the coldest
Obtain graphene oxide serosity the most afterwards；Low-temperature heat temperature is 60-70 DEG C, and heat time heating time is 30-50min；
Step 4, carries out neutral cleaning, until in neutrality, being configured to graphene aqueous solution after drying by graphene oxide serosity；Institute
Stating drying temperature and be 80-100 DEG C, drying time is 20-30min；
Step 5, adds the first modifying agent, penetrating agent, the second dispersant in graphene aqueous solution, carries out water-bath backflow, obtain
Deep layer modified graphene solution；Described bath temperature is 90-105 DEG C, and return time is 60-120min；
Step 6, after carrying out deep layer modified graphene solution filtering cleaning, dries and obtains deep layer modified graphene powder body；
Step 7, puts in ethanol solution by deep layer modified graphene powder body, adds the second modifying agent, acid solution, ultrasonic resonance,
Clean to neutral after filtration, after drying, i.e. can get modified graphene powder body；Described supersonic frequency is 10-15MHz, described ultrasonic
Time is 20-35min；
Step 8, steams after modified graphene powder body, silicones, metal-oxide, levelling agent, Polyethylene Glycol mix and blend
Send to be formed thick, then carry out high temperature sintering, i.e. can get modified graphene material；Described evaporating temperature is 100-110
DEG C, high temperature sintering temperature is 300-500 DEG C, sintering time 300-480min.
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Cited By (1)
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Application publication date: 20170104 |